CN101845624B - Method for preparing alkaline nano-zirconium carbide composite nickel-phosphorus coating on surface of polyester fabric - Google Patents
Method for preparing alkaline nano-zirconium carbide composite nickel-phosphorus coating on surface of polyester fabric Download PDFInfo
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- CN101845624B CN101845624B CN2010101954112A CN201010195411A CN101845624B CN 101845624 B CN101845624 B CN 101845624B CN 2010101954112 A CN2010101954112 A CN 2010101954112A CN 201010195411 A CN201010195411 A CN 201010195411A CN 101845624 B CN101845624 B CN 101845624B
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Abstract
The invention discloses a method for preparing an alkaline nano-zirconium carbide composite nickel-phosphorus coating on the surface of a polyester fabric, which comprises the following steps of: pre-treating the polyester fabric, which comprises the steps of coarsening, sensitized activation, peptization and reduction; and plating the polyester fabric, which comprises the steps of weighting and mixing nana-dispersion and Ni-P electroless plating solution in the volume ratio of (0.03 to 0.05):1 so as to obtain plating solution, heating the plating solution, and immersing the polyester fabric subjected to pretreatment into the plating solution at the temperature of 60 to 70 DEG C to carry out plating reaction for 30 to 40 minutes so as to complete the process of preparing an alkaline nano-zirconium carbide composite nickel-phosphorus coating on the surface of the polyester fabric. According to the method, a dispersing agent Tween 80 is used to carry out ultrasonic oscillation so as to fully disperse the nano-zirconium carbide particles, and then the nano-zirconium carbide particles are added in the alkaline Ni-P solution, so that the nano-zirconium carbide particles are steadily dispersed in the Ni-P solution, the plated coating structure of the polyester fabric is compact, and the wear-resisting performance and washable performance of the polyester alkaline electroless Ni-P fabrics are 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 treatment method of polyester piece good, be specifically related to a kind of method at polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating.
Background technology
The chemical nickel phosphorus plating fabric had both kept original fabric sofetening, gas-pervious style; Given the characteristic of fabric conduction and electromagnetic wave shielding again; Can be made into account, curtain and wall paper and be used for the place in computer house and other applied microwave sources; Guarantee that electronics normally moves, reduce the pollution of hertzian wave environment; Also can be sewn into clothes, gloves and cap makes the staff avoid the irradiation of electromagnetic waves injury; Surperficial heating unit be can also process and the surface heating of particular device and the resisting cold insulation of severe cold area are used for; While chemical nickel phosphorus plating fabric is reflection of electromagnetic wave efficiently and sound insulation packing material still, therefore is widely used in fields such as national defence, Aeronautics and Astronautics, electronics, electric power, communication and medical treatment, is a kind of important function property textile materials.
Existing chemical plating nickel-phosphorus alloy preparation process of textile; The nano particle that adopts has zinc oxide, silit and tindioxide; Use sodium alginate soln to carry out ultra-sonic dispersion, and then nano dispersion fluid is added in the chemical nickel phosphorus plating liquid, prepare nano particle chemical composite nickel-plating phosphorus fabric as dispersion liquid; Nanoparticulate dispersed is bad in the plating bath; Nano particle can not be individual particle and be dispersed in the plating bath, so the bonding force of coating and fibrous matrix is poor, has had a strong impact on wear-resisting, the washing resistance performance of chemical nickel phosphorus plating fabric.
Summary of the invention
The purpose of this invention is to provide a kind of method, solved the wear-resisting and relatively poor problem of washing resistance performance of existing chemical nickel phosphorus plating fabric at polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating.
The technical scheme that the present invention adopts is, a kind of method at polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating is specifically implemented according to following steps:
Step 1: polyester piece good pre-treatment: alligatoring, sensitizing and activating, dispergation, reduction;
Step 2: plating polyester piece good: according to volume ratio is that 0.03～0.15:1 takes by weighing nano dispersion fluid and chemical nickel plating phosphorus solution; Mix and obtain plating bath; The heating plating bath, when bath temperature reached 60～70 ℃, the polyester piece good after the pre-treatment that step 1 is obtained immersed and carries out the plating reaction in the plating bath; Reaction times 30～40min promptly accomplishes at polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating.
Characteristics of the present invention also are,
The nano dispersion fluid in the step 2 wherein; Be to be to add the nano-zirconium carbide particle in the tween 80 solution of 0.5～2.5g/L to obtain mixing solutions to quality-volumetric concentration; Quality-the volumetric concentration of nano-zirconium carbide is 0.5～2g/L in the mixing solutions; Is 28～50KHz with mixing solutions in frequency, and power is that sonic oscillation 10～30min is prepared under the condition of 100～200W.
The chemical nickel plating phosphorus solution in the step 2 wherein; It consists of according to quality-volumetric concentration: the Trisodium Citrate of the single nickel salt of 25～35g/L, the sodium hypophosphite of 25～35g/L, 15～25g/L and the ammonium chloride of 20～30g/L, the pH value of chemical nickel plating phosphorus solution is 7～9.
The wherein alligatoring in the step 1, specifically implement according to following steps: adopt quality-volumetric concentration be the sodium hydroxide solution of 160～240g/L as coarsening solution, polyester piece good is placed in the coarsening solution, be under 60～90 ℃ the condition, to handle 15～40min in temperature.
The sensitizing and activating in the step 1 wherein; Specifically implement: with the polyester piece good after the alligatoring according to following steps; Being placed in the colloidal pd activation solution, is under 50～70 ℃ of conditions in temperature, handles 2～6 hours; 1.0～4.0, it consists of colloidal pd activation solution according to quality-volumetric concentration: the hydrochloric acid of the Palladous chloride of 0.12～0.20g/L, the tin protochloride of 8～14g/L, 9.5～16.5g/L and the sodium-chlor of 140～180g/L with hydrochloric acid control reaction pH value.
The dispergation in the step 1 wherein, specifically implement according to following steps: the polyester piece good after the sensitizing and activating being placed on separating in the glue, is under 35～55 ℃ the condition, to handle 1～5min in temperature, separating glue, to adopt quality-volumetric concentration be the hydrochloric acid of 95～140g/L.
The wherein reduction in the step 1, specifically implement according to following steps: the polyester piece good behind the dispergation is placed in the reduced liquid, at ambient temperature, handles 2～8min, it is the sodium hypophosphite solution of 10～20g/L that reduced liquid adopts quality-volumetric concentration.
The invention has the beneficial effects as follows; On the basis of traditional alkaline chemical nickel-plating phosphorus technology; Polyester piece good is carried out nano-zirconium carbide particle composite nickel-plating phosphorus handle,, select for use the dispersion agent tween 80 that the nano-zirconium carbide particle is disperseed to the easy shortcoming of reuniting of nano-zirconium carbide particle; And it is added in the alkaline chemical nickel-plating liquid; Improve the dispersion stabilization of nano-zirconium carbide particle in plating bath, strengthened the bonding strength between nano particle and the coating, thereby improved the wear-resisting and washing resistance performance of coating.
Description of drawings
Fig. 1 is the stereoscan photograph of common alkaline nickel plating phosphorus polyester piece good;
Fig. 2 is the stereoscan photograph that adopts the alkaline nano-zirconium carbide composite nickel-plating phosphorus polyester piece good of the inventive method preparation;
Fig. 3 is the X-ray energy spectrum figure of common alkaline nickel plating phosphorus polyester piece good;
Fig. 4 is the X-ray energy spectrum figure that adopts the alkaline nano-zirconium carbide composite nickel-plating phosphorus polyester piece good of the inventive method preparation.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
The present invention specifically implements according to following steps in the method for polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating:
Step 1: polyester piece good pre-treatment.Before nickel plating phosphorus, must carry out a series of pre-treatments, make fiber surface have catalytic activity and hackly C.E., increase the contact area of coating and fiber, so that bring out electroless plating reaction and obtain the good coating of bonding force to polyester piece good.Pre-treatment is specifically implemented according to following steps:
A. alligatoring, adopt quality-volumetric concentration be the sodium hydroxide solution of 160～240g/L as coarsening solution, polyester piece good is placed in the coarsening solution, be under 60～90 ℃ the condition, to handle 15～40min in temperature.
The purpose of alligatoring is nano and micro relief and the contact area that increases PET fiber surface, guarantees that nickel-phosphorus coating has good sticking power, improves the bonding strength of metal and fiber surface.Alligatoring will change the microcosmos geometric shape and the macromolecular chemical property of fiber surface, possess wetting ability thereby form polar group at fiber surface, help combining of fiber and nickel phosphorus gold genus.Weight-loss ratio is the key factor that influences coating adhesion, and along with the increase of weight-loss ratio, losing largely can appear in fabric strength.Guaranteeing that weight-loss ratio is controlled between 8～16% under the prerequisite that coating adhesion acquires a certain degree and strength loss is not too large.
B. sensitizing and activating, the polyester piece good 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, maintain 1.0～4.0 with hydrochloric acid control reaction pH value; Colloidal pd activation solution is prepared according to quality-volumetric concentration, and it consists of: Palladous chloride 0.12～0.20g/L, tin protochloride 8～14g/L; Hydrochloric acid 9.5～16.5g/L, sodium-chlor 140～180g/L.
Sensitizing and activating is the polyester piece good of alligatoring to be put into sensitizing solution flood, and tindihydroxide or tin protoxide that the tin salt hydrolysis is generated are deposited on fiber surface.Stannous ion is reduced into the palladium metal particle to the palladium ion in the activation solution, under the fiber surface deposition, forms metallic palladium crystal grain or metallic membrane, and this tunic plays the effect of catalyzer, and electroless plating reaction is accelerated.For keeping the stability of activation solution; Make the catalytic activation center of fiber surface absorption tiny, fine and close; Guarantee that fiber surface coating is even, the content of Palladous chloride is low a little in the activation solution, adopts the mode that slowly drips under the high-speed stirring condition can obtain good activation effect.
C. dispergation, the polyester piece good 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 95～140g/L.
Dispergation is to select certain density hydrochloric acid soln for use, and the divalence or the tetravalent tin ion of dissolving partly hydrolysed expose the palladium metal particulate with catalytic activity, to reach the activatory effect.
D. reduction, the polyester piece good behind the dispergation that the last step was obtained is placed in the reduced liquid, at ambient temperature, handles 2～8min.It is the sodium hypophosphite solution of 10～20g/L that reduced liquid adopts quality-volumetric concentration.
Reduction is that the fabric behind the dispergation is immersed in the reduced liquid, makes palladium ion be reduced into metal particle and is deposited on fiber surface.
Step 2: plating polyester piece good.
Preparation chemical nickel plating phosphorus solution: according to quality-volumetric concentration; Take by weighing the single nickel salt of 25～35g/L; The sodium hypophosphite of 25～35g/L, the Trisodium Citrate of 15～25g/L, the ammonium chloride of 20～30g/L; Mix the water-soluble chemical nickel plating phosphorus solution for preparing in back, the pH value of using ammoniacal liquor to regulate the chemical nickel plating phosphorus solution is 7～9.
The preparation of nano dispersion liquid: to quality-volumetric concentration is to add the nano-zirconium carbide particle in the tween 80 solution of 0.5～2.5g/L; Make the quality-volumetric concentration of nano-zirconium carbide at 0.5～2g/L; In frequency is 28～50KHz; Power is sonic oscillation 10～30min under the condition of 100～200W, obtains nano dispersion fluid.
The preparation plating bath: according to volume ratio is 0.03～0.15:1, and nano dispersion fluid is slowly added in the chemical nickel plating phosphorus solution, in this process, constantly stirs, and obtains plating bath.
Put into water-bath to plating bath then and heat, when bath temperature reached 60～70 ℃, the polyester piece good that step 1 is obtained immersed and carries out the plating reaction in the plating bath; Reaction times 30～40min; Treat that plating bath becomes clear, take out the good polyester piece good of plating, water cleans repeatedly; Naturally dry, promptly accomplish at polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating.
According to standard GB/T 21196.3-2007 " mensuration the 3rd part of textiles Martindale fabric abrasion resistance: mass loss confirm ", GB/T 21196.4-2007 " mensuration the 4th part of textiles Martindale fabric abrasion resistance: the evaluation of cosmetic variation ", detect the wear resisting property of the alkaline composite nickel-plating phosphorus of alkaline nickel plating phosphorus fabric and nano-zirconium carbide fabric.Abrasive material is selected woven plain weave wool fabric for use, and friction load is 795 ± 7g.When rate of body weight gain 80～150% the time, through after 15000 plain grindings, alkaline nickel plating phosphorus fabric quality rate of loss is 8～18%, and alkaline nano-zirconium carbide composite nickel-plating phosphorus fabric quality rate of loss is 2～4%; When fabric reaches friction terminal point (obviously printing opacity); The diffusive that promptly the adds up area that comes off fully reaches 1/3rd when above; Alkalescence nickel plating phosphorus fabric friction number of times is 25000～38000 times, and alkaline nano-zirconium carbide composite nickel-plating phosphorus fabric friction number of times is 35000～55000 times.
According to textile industry standard FZ/T 60014-1993 " mensuration of metallised textile article and the durable scourability of flocculus ", detect the washing resistance performance of alkaline nickel plating phosphorus fabric and nano-zirconium carbide composite nickel-plating phosphorus.Specimen size is 10cm * 10cm, and at bath raio 1:40, standard wash agent consumption lg/L washs under 2 ℃ of conditions of temperature 40 scholars.When the fabric rate of body weight gain 80～150% the time, after 20 washings, the coating of alkaline nickel plating phosphorus fabric and alkaline nano-zirconium carbide composite nickel-plating phosphorus fabric the big area diffusive all do not occur and comes off.
Fig. 1 and Fig. 2 are respectively the stereoscan photograph of common alkaline nickel plating phosphorus polyester piece good and the stereoscan photograph of the alkaline nano-zirconium carbide composite nickel-plating phosphorus polyester piece good that the inventive method prepares; As can be seen from the figure; Common alkaline nickel plating phosphorus coating surface is relatively smooth, clean; After the adding nano-zirconium carbide particle (150ml/L), alkaline nano-zirconium carbide composite nickel-plating phosphorus coating surface cosmetic variation is little, but hole obviously reduces.
Fig. 3 and Fig. 4 are respectively the X-ray energy spectrum figure of common alkaline nickel plating phosphorus polyester piece good and the X-ray energy spectrum figure that adopts the alkaline nano-zirconium carbide composite nickel-plating phosphorus polyester piece good of the inventive method preparation; As can be seen from the figure; Common alkaline nickel plating phosphorus coating contains nickel and two kinds of elements of phosphorus, and wherein the nickel element massfraction is 98.3%, and atomic fraction is 96.8%; The phosphoric massfraction is 1.7%, and atomic fraction is 3.2%; Alkaline nano-zirconium carbide particle compound plating nickel-phosphorus coating contains nickel, phosphorus and three kinds of elements of zirconium, and wherein the nickel element massfraction is 96.6%, and atomic fraction is 95.0%; The phosphoric massfraction is 2.3%; Atomic fraction is 4.2%, and the zr element massfraction is 1.1%, and atomic fraction is 0.8%.Increased zr element; Show and contain the nano-zirconium carbide composition in the metal plating; And that nano-zirconium carbide material has is high temperature resistant, anti-oxidant, intensity is high, hardness is high, thermal conductivity is good, and many advantages such as good toughness are a kind of important HMP, HS and corrosion resistant high-temperature structural material; And have efficient absorption visible light, characteristics such as reflected infrared and energy storage.The nano-zirconium carbide particle can " be filled up " hole that coating forms owing to liberation of hydrogen, can spread with the atoms metal in the coating, perhaps forms coordination absorption even chemically bonded, thereby improves the density of coating, improves wear resisting property.
Beneficial effect of the present invention place is described from the principle aspect:
1. the present invention adopts the nano-zirconium carbide particle, controls its quality-volumetric concentration at 0.5～2g/L.When greater than this scope, nano-zirconium carbide concentration increases, and the nano particle showed increased that unit volume contained in solution is prone to cause reunion, forms deposition, also is prone to cause waste; When less than this scope, when in chemical nickel phosphorus plating liquid, adding nano dispersion fluid, the nano-dispersed liquid measure of adding is just more relatively, and destructible plating bath internal medium influences electroless plating reaction, and fabric is plating normally.
2. the dispersion agent of the present invention's employing is a tween 80; Tween 80 is the mixture of Tween 80 and the two sorbitol monooleates that anhydrate of a part of T 46155; Soluble in water; Main as emulsifying agent, when tween 80 quality-volumetric concentration during at 0.5～2.5g/L, the nano-zirconium carbide dispersion stabilization is good; When greater than this scope, tween 80 concentration is excessive, can influence electroless plating carries out smoothly after joining in the plating bath, and the influence of plating speed is obvious; When less than this scope, do not reach nano-zirconium carbide particle well stabilized and disperse.
3. the volume ratio of nano dispersion fluid and chemical nickel plating phosphorus solution is 0.03～0.15:1 in the plating bath, and when greater than this scope, the nano-zirconium carbide consumption increases relatively, the one, and serious waste phenomenon, the 2nd, it is very unstable that plating bath becomes, and influences the plating smooth implementation; When less than this scope, the nano-zirconium carbide consumption is less relatively, be deposited in the coating nano-zirconium carbide content seldom, do not reach the purpose that strengthens coating structure.
Embodiment 1
Selecting 160g/L sodium hydroxide for use, is under 60 ℃ of conditions polyester piece good to be carried out roughening treatment 15 min in temperature, and the control weight-loss ratio is 8%.Select the 0.12g/L Palladous chloride for use, the 8g/L tin protochloride, 9.5g/L hydrochloric acid, 140g/L sodium-chlor, the pH value is 1.0, is to carry out the colloidal palladium activation treatment 2 hours under 50 ℃ of conditions in temperature.Select 95g/L hydrochloric acid for use, under 35 ℃ of conditions of temperature, carry out dispergation and handle 1min.Select the 10g/L sodium hypophosphite for use, reduce at ambient temperature and handle 2min.The chemical nickel phosphorus plating solution formula is: the 25g/L single nickel salt, and the 25g/L sodium hypophosphite, the 15g/L Trisodium Citrate, 20g/L ammonium chloride, using ammoniacal liquor to regulate the pH value is 7, temperature is 60 ℃.In the tween 80 solution of 0.5g/L, add the nano-zirconium carbide particle, control nano-zirconium carbide quality-volumetric concentration at 0.5g/L, sonic oscillation 10min under frequency 28KHz power 100W condition; Slowly join in chemical nickel-plating liquid by the consumption of 30ml/L scattered nano dispersion fluid again; The good polyester piece good that under 60 ℃ of conditions, will reduce immerses and carries out the plating reaction in the nano combined plating bath; Treat to take out polyester piece good behind the 30min, clean repeatedly, dry naturally with tap water.
Detect nickel plating phosphorus fabric abrasion resistance ability according to standard GB/T 21196.3-2007 and GB/T 21196.4-2007.Abrasive material is selected woven plain weave wool fabric for use, and friction load is 795 ± 7g.When rate of body weight gain is 80%, through after 15000 plain grindings, alkaline nickel plating phosphorus fabric quality rate of loss is 17.8%, and alkaline nano-zirconium carbide composite nickel-plating phosphorus fabric quality rate of loss is 3.9%; When fabric reached friction terminal point (obviously printing opacity), alkaline nickel plating phosphorus fabric friction number of times was 25300 times, and alkaline nano-zirconium carbide composite nickel-plating phosphorus fabric friction number of times is 35400 times.Detect the washing resistance performance of common nickel plating phosphorus fabric and nano-zirconium carbide composite nickel-plating phosphorus according to textile industry standard FZ/T 60014-1993.Specimen size is 10cm * 10cm, and at bath raio 1:40, standard wash agent consumption 1g/L washs under 40 ℃ of conditions of temperature.When the fabric rate of body weight gain 80% the time, after 20 washings, common nickel plating phosphorus fabric and nano-zirconium carbide composite nickel-plating phosphorus fabric coating the big area diffusive all do not occur and come off.
Selecting 240g/L sodium hydroxide for use, is under 90 ℃ of conditions polyester piece good to be carried out roughening treatment 40min in temperature, and the control weight-loss ratio is 16%.Select the 0.20g/L Palladous chloride for use, the 14g/L tin protochloride, 16.5g/L hydrochloric acid, 180g/L sodium-chlor, the pH value is 1.4, is to carry out the colloidal palladium activation treatment 6 hours under 70 ℃ of conditions in temperature.Select 140g/L hydrochloric acid for use, under 55 ℃ of conditions of temperature, carry out dispergation and handle 5min.Select the 20g/L sodium hypophosphite for use, reduce at ambient temperature and handle 8min.The chemical nickel phosphorus plating solution formula is: the 35g/L single nickel salt, and the 35g/L sodium hypophosphite, the 25g/L Trisodium Citrate, 30g/L ammonium chloride, using ammoniacal liquor to regulate the pH value is 9,70 ℃ of temperature.In the tween 80 solution of 2.5g/L, add the nano-zirconium carbide particle, control nano-zirconium carbide quality-volumetric concentration at 2.0g/L, sonic oscillation 30min under frequency 50KHz power 200W condition; Slowly join in chemical nickel-plating liquid by the 150ml/L consumption scattered nano dispersion fluid again; The good polyester piece good that under 70 ℃ of conditions, will reduce immerses and carries out the plating reaction in the nano combined plating bath; Treat to take out the plating polyester piece good behind the 40min, clean repeatedly, dry naturally with tap water.
Detect nickel plating phosphorus fabric abrasion resistance ability according to standard GB/T 21196.3-2007 and GB/T 21196.4-2007.Abrasive material is selected woven plain weave wool fabric for use, and friction load is 795 ± 7g.When rate of body weight gain is 150%, through after 15000 plain grindings, alkaline nickel plating phosphorus fabric quality rate of loss is 7.6%, and alkaline nano-zirconium carbide composite nickel-plating phosphorus fabric quality rate of loss is 2.2%; When fabric reached friction terminal point (obviously printing opacity), alkaline nickel plating phosphorus fabric friction number of times was 37500 times, and alkaline nano-zirconium carbide composite nickel-plating phosphorus fabric friction number of times is 54800 times.Detect the washing resistance performance of common nickel plating phosphorus fabric and nano-zirconium carbide composite nickel-plating phosphorus according to textile industry standard FZ/T 60014-1993.Specimen size is 10cm * 10cm, and at bath raio 1:40, standard wash agent consumption lg/L washs under 40 ℃ of conditions of temperature.When the fabric rate of body weight gain 150% the time, after 20 washings, common nickel plating phosphorus fabric and nano-zirconium carbide composite nickel-plating phosphorus fabric coating the big area diffusive all do not occur and come off.
Selecting 200g/L sodium hydroxide for use, is under 80 ℃ of conditions polyester piece good to be carried out roughening treatment 30 min in temperature, and the control weight-loss ratio is 12%.Select the 0.15g/L Palladous chloride for use, the 12g/L tin protochloride, 12g/L hydrochloric acid, 160g/L sodium-chlor, pH value 4.0 is to carry out the colloidal palladium activation treatment 5 hours under 60 ℃ of conditions in temperature.Select 130g/L hydrochloric acid for use, under 40 ℃ of conditions of temperature, carry out dispergation and handle 3min.Select the 15g/L sodium hypophosphite for use, reduce at ambient temperature and handle 5min.The chemical nickel phosphorus plating solution formula is: the 30g/L single nickel salt, and the 30g/L sodium hypophosphite, the 20g/L Trisodium Citrate, 25g/L ammonium chloride, using ammoniacal liquor to regulate the pH value is 8,65 ℃ of temperature.In the tween 80 solution of 2.0g/L, add the nano-zirconium carbide particle, control zirconium carbide quality-volumetric concentration at 1.5g/L, at frequency 30KHz, sonic oscillation 15min under the power 150W condition; Slowly join in chemical nickel-plating liquid by the 80ml/L consumption scattered nano dispersion fluid again; The good polyester piece good that under 65 ℃ of conditions, will reduce immerses and carries out the plating reaction in the nano combined plating bath; Take out polyester piece good behind the question response 35min, clean repeatedly, dry naturally with tap water.
Detect nickel plating phosphorus fabric abrasion resistance ability according to standard GB/T 21196.3-2007 and GB/T 21196.4-2007.Abrasive material is selected woven plain weave wool fabric for use, and friction load is 795 ± 7g.When rate of body weight gain is 120%, through after 15000 plain grindings, alkaline nickel plating phosphorus fabric quality rate of loss is 9.1%, and alkaline nano-zirconium carbide composite nickel-plating phosphorus fabric quality rate of loss is 2.4%; When fabric reached friction terminal point (obviously printing opacity), alkaline nickel plating phosphorus fabric friction number of times was 30600 times, and alkaline nano-zirconium carbide composite nickel-plating phosphorus fabric friction number of times is 42800 times.Detect the washing resistance performance of common nickel plating phosphorus fabric and nano-zirconium carbide composite nickel-plating phosphorus according to textile industry standard FZ/T 60014-1993.Specimen size is 10cm * 10cm, and at bath raio 1:40, standard wash agent consumption lg/L washs under 40 ℃ of conditions of temperature.When the fabric rate of body weight gain 120% the time, after 20 washings, common nickel plating phosphorus fabric and nano-zirconium carbide composite nickel-plating phosphorus fabric coating the big area diffusive all do not occur and come off.
The present invention is in the method for polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating; Use the abundant dispersing nanometer zirconium carbide particle of dispersion agent tween 80 sonic oscillation; Then it is added in the alkaline chemical nickel-plating liquid; Make nano-zirconium carbide particle stable dispersion in nickel-plating liquid, the polyester piece good coating structure of plating is tight, improves the wear-resisting and washing resistance performance of terylene alkalescence nickel plating phosphorus fabric.
Claims (6)
1. the method at polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating is characterized in that, specifically implements according to following steps:
Step 1: polyester piece good pre-treatment: alligatoring, sensitizing and activating, dispergation, reduction;
Step 2: plating polyester piece good: according to volume ratio is that 0.03～0.15:1 takes by weighing nano dispersion fluid and chemical nickel plating phosphorus solution; Mix and obtain plating bath; Described nano dispersion fluid; Be to be to add the nano-zirconium carbide particle in the tween 80 solution of 0.5～2.5g/L to obtain mixing solutions to quality-volumetric concentration; Quality-the volumetric concentration of nano-zirconium carbide is 0.5～2g/L in the mixing solutions, is 28～50KHz with mixing solutions in frequency, and power is that sonic oscillation 10～30min is prepared under the condition of 100～200W; The heating plating bath, when bath temperature reached 60～70 ℃, the polyester piece good after the pre-treatment that step 1 is obtained immersed and carries out the plating reaction in the plating bath, and reaction times 30～40min promptly accomplishes at polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating.
2. the method at polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating according to claim 1; It is characterized in that; Chemical nickel plating phosphorus solution in the described step 2; It consists of according to quality-volumetric concentration: the Trisodium Citrate of the single nickel salt of 25～35g/L, the sodium hypophosphite of 25～35g/L, 15～25g/L and the ammonium chloride of 20～30g/L, the pH value of chemical nickel plating phosphorus solution is 7～9.
3. the method at polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating according to claim 1; It is characterized in that; Alligatoring in the said step 1, specifically implement according to following steps: adopt quality-volumetric concentration be the sodium hydroxide solution of 160～240g/L as coarsening solution, polyester piece good is placed in the coarsening solution; Be under 60～90 ℃ the condition, to handle 15～40min in temperature.
4. the method at polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating according to claim 1; It is characterized in that; Sensitizing and activating in the said step 1 is specifically implemented according to following steps: with the polyester piece good after the alligatoring, be placed in the colloidal pd activation solution; In temperature is under 50～70 ℃ of conditions; Handled 2～6 hours, 1.0～4.0, it consists of colloidal pd activation solution according to quality-volumetric concentration: the hydrochloric acid of the Palladous chloride of 0.12～0.20g/L, the tin protochloride of 8～14g/L, 9.5～16.5g/L and the sodium-chlor of 140～180g/L with hydrochloric acid control reaction pH value.
5. the method at polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating according to claim 1; It is characterized in that; Dispergation in the said step 1, specifically implement according to following steps: the polyester piece good after the sensitizing and activating being placed on separating in the glue, is under 35～55 ℃ the condition in temperature; Handle 1～5min, separating glue employing quality-volumetric concentration is the hydrochloric acid of 95～140g/L.
6. the method at polyester piece good surface preparation alkaline nano-zirconium carbide composite nickel-phosphorus coating according to claim 1; It is characterized in that; Reduction in the said step 1 is specifically implemented according to following steps: the polyester piece good behind the dispergation is placed in the reduced liquid, at ambient temperature; Handle 2～8min, it is the sodium hypophosphite solution of 10～20g/L that reduced liquid adopts quality-volumetric concentration.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101954112A CN101845624B (en) | 2010-06-09 | 2010-06-09 | Method for preparing alkaline nano-zirconium carbide composite nickel-phosphorus coating on surface of polyester fabric |
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| CN2010101954112A CN101845624B (en) | 2010-06-09 | 2010-06-09 | Method for preparing alkaline nano-zirconium carbide composite nickel-phosphorus coating on surface of polyester fabric |
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| CN101845624A CN101845624A (en) | 2010-09-29 |
| CN101845624B true CN101845624B (en) | 2012-08-22 |
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| CN102154818B (en) * | 2011-05-16 | 2012-05-09 | 东北林业大学 | Method for preparing nickel coating on surface of cotton fabric or linen fabric |
| CN103469180A (en) * | 2013-09-16 | 2013-12-25 | 苏州志向纺织科研股份有限公司 | Method for preparing antistatic polyester through chemical nickel-plating process |
| CN103556137B (en) * | 2013-11-07 | 2015-10-28 | 杭州东方表面技术有限公司 | A kind of environmental-protecting chemical for metallization of plastic surface modification sinks nickel solution |
| CN105063579B (en) * | 2015-07-20 | 2017-12-08 | 深圳市瑞世兴科技有限公司 | The coarsening solution and its plating nickel on surface method of diamond carbon/carbon-copper composite material |
| 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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| 刘荣立等.涤纶织物化学复合镀（Ni-P）-SnO2纳米微粒复合镀层.《电镀与精饰》.2008,第30卷(第8期),29-32. * |
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