CN102515778A - Electroconductive woodceramic powder and its manufacturing method - Google Patents
Electroconductive woodceramic powder and its manufacturing method Download PDFInfo
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Abstract
Relating to woodceramic materials and their preparation methods, the invention provides electroconductive woodceramic powder and its manufacturing method, and solves the technical problems of great brittleness and easy cracking in bulk woodceramic materials. The electroconductive woodceramic powder of the takes woodceramic powder as the core, the surface of which is chemically plated with electroconductive powder of a layer of metal film, and the metal attaching amount is 1%-50% of the mass of the woodceramic powder, wherein, the metal is nickel, iron or cobalt. The preparation method consists of: subjecting the woodceramic powder to oil removal, oxidation, sensitization, activation, and dispergation, then placing the woodceramic powder into a chemical plating solution for chemical plating, and conducting filtration and washing by deionized water to neutral, then carrying out drying, thus obtaining the electroconductive woodceramic powder with volume resistivity of 4.5*10<-2>omega.cm-5.5*10<-1>omega.cm. The electroconductive woodceramic powder in the invention can be added into coatings for preparing electroconductive coatings, or the powder can be added into resin-based materials for preparing molding materials, thus having a wide application range. The electroconductive woodceramic powder in the invention can be used as an electromagnetic shielding material.
Description
Technical field
The present invention relates to wooden stupalith and preparation method thereof.
Background technology
All electrical equipments all can generate electromagnetic waves when operation, cause electromagnetic radiation.The electromagnetic radiation meeting works the mischief to instrument, equipment, and HUMAN HEALTH is also had detrimentally affect, and oneself classifies electromagnetic pollution as after topsoil, water pollution, sound pollution the fourth-largest public hazards by warp the World Health Organization.Existing research shows that the harm of electromagnetic radiation mainly contains: (1) harm information security makes instrument such as computingmachine not have security assurance information.(2) highly sophisticated device equipment implementation is caused serious interference.(3) harm humans is healthy.Can give rise to diseases when electromagnetic pollution is serious.Therefore, need ensure information security, avoid the place and the equipment of electromagnetic radiation to some, adopting electromangnetic spectrum is vital preventive measures.Electromagnet shield effect depends primarily on shielding material to absorption of electromagnetic wave and reflection.
The wood pottery be by wood materials dipping or not behind the heat of immersion thermosetting resin under the condition of secluding air; Porous biological matter raw material of wood-charcoal material through high temperature sintering forms has the certain electromagnetic shielding properties, and publication number is the preparation method that the Chinese patent of CN1970260A discloses a kind of reinforced wood ceramic; Behind the xylon solvent impregnated resin; Be mixed with strengthening material, after compacting, the bulk material that sintering obtains.This wood pottery has electromagnetic performance preferably, but because its fragility is bigger, is very easy to cracking when sintering is made the large size product, is difficult in the industrial circle widespread use.
Summary of the invention
The present invention will solve the wooden stupalith fragility of existing bulk technical problem big, easy to crack, and wooden ceramics powder of a kind of conduction and method of manufacture thereof are provided.
The wooden ceramics powder of a kind of conduction of the present invention is to be core body with wooden ceramics powder, and at the conductive powder body of core surface chemical plating layer of metal film, the adhesion amount of metal is 1%～50% of a wooden ceramics powder quality; Wherein metal is nickel, iron or cobalt.
Wherein the preparation method as the wooden ceramics powder of core body is undertaken by following: be to be dried to over dry under 30 ℃～100 ℃ the condition in temperature with biomass material; Then with the exsiccant biomass material under vacuum environment or protection of inert gas; At 600 ℃～2500 ℃ sintering 2h～10h of temperature; Be crushed to granularity 0.1 μ m～200 μ m with ball mill again, obtain wooden ceramics powder as core body; Wherein biomass material is timber, nut-shell, bamboo wood, rice husk, coffee grounds, tea grounds, tobacco rod, bagasse, xylogen or waste paper.
Preparing method as the wooden ceramics powder of core body can also carry out according to the following steps: a, with biomass material be immersed in keep 20h～30h in the resin after; Biomass material is filtered out; And be that to be dried to water ratio under 30 ℃～100 ℃ the condition be 1%～3% in temperature, obtain dried particles; Again dried particles being placed on temperature is to keep 6h～10h in 180 ℃～220 ℃ the baking oven, obtains cured granulate; B, under vacuum environment or protection of inert gas, at 600 ℃～2500 ℃ sintering 2h～10h of temperature, using ball mill to be crushed to granularity again is 0.1 μ m～200 μ m, obtains the wooden ceramics powder as core body with the cured granulate of step a preparation; Wherein biomass material is timber, nut-shell, bamboo wood, rice husk, coffee grounds, tea grounds, tobacco rod, bagasse, xylogen or waste paper among the step a; Wherein the resin among the step a is resol, epoxy resin, urethane, polysulfone resin or polyimide resin.
A kind of preparation method of conducting electricity wooden ceramics powder of the present invention carries out according to the following steps:
One, join wooden ceramics powder in organic solvent or the tensio-active agent, ultra-sonic dispersion 10min～15min filters out wooden ceramics powder then, after deionized water wash, drying, obtains clean wooden ceramics powder;
It is to stir 10min～15min in 60%～65% the concentrated nitric acid solution that the wooden ceramics powder of the cleaning that two, step 1 is obtained joins mass percent concentration; Then wooden ceramics powder is filtered out; To neutrality, drying, obtain the wooden ceramics powder of surface oxidation with deionized water rinsing;
Three, being that 37% hydrochloric acid is solvent with mass percentage concentration, is that 10g/L is dissolved in tin protochloride in the hydrochloric acid solvent by the concentration of tin protochloride, obtains stannous chloride solution; The wooden ceramics powder of the surface oxidation that step 2 is obtained is added in the stannous chloride solution; Be to stir 30min～45min under 50 ℃～60 ℃ the condition in temperature; Then wooden ceramics powder is filtered out, after deionized water wash, drying, obtain sensitization wood ceramics powder;
Four, the sensitization wood ceramics powder that step 3 is obtained joins in the colloidal pd activation solution; Be to stir 20min～30min under 35 ℃～50 ℃ the condition in temperature, after wooden ceramics powder is filtered out, join in the concentrated hydrochloric acid; Be to stir 1min～3min under 40 ℃ the condition in temperature; Again wooden ceramics powder is filtered out, after deionized water wash, drying, obtain the wooden ceramics powder of surperficial pre-treatment;
The wooden ceramics powder of the surperficial pre-treatment that five, step 4 is obtained joins and keeps 40min～50min in the chemical plating fluid, then through filtering, after deionized water wash to neutral, the drying, obtaining conducting electricity wooden ceramics powder.
Tensio-active agent in the step 1 can be an anionic or/and non-ionics, and organic solvent is with acetone or methylethyl copper;
Wherein colloidal pd activation solution is that concentration by Palladous chloride is that the concentration of 1.0g/L, tin protochloride is that 70g/L, mass percent concentration are the concentration 300mL/L of 37% hydrochloric acid in the step 4, is that 37% hydrochloric acid is added to the water formulated with Palladous chloride, tin protochloride and mass percent concentration; Concentrated hydrochloric acid in the step 4 is that mass percent is 37% concentrated hydrochloric acid.
It is formulated that chemical plating solution in the step 5 is that the concentration by main salt is that the concentration of 35g/L～50g/L, sodium laurylsulfonate is that the concentration of 3g/L～5g/L, sodium hypophosphite is that the concentration of 70g/L～85g/L, Trisodium Citrate is that the concentration of 80g/L～100g/L, ammonium chloride is that the concentration of 100g/L～120g/L, lead sulfate is that 2mg/L～4mg/L is added to the water main salt, sodium laurylsulfonate, sodium hypophosphite, Trisodium Citrate, ammonium chloride and lead sulfate, and wherein main salt is single nickel salt, ferric sulfate, rose vitriol, nickelous chloride, iron(ic)chloride or NSC 51149;
Wooden ceramics powder of the present invention is a kind of nanometer, micron-sized powder, has vesicular structure, and specific surface area is big; Be difficult in water, disperse, though have electroconductibility, its surface does not have the function of catching metals ion; Therefore be difficult to directly at its coating surface metallic membrane, therefore, the present invention has adopted a kind of pre-treating technology; Promptly earlier remove buoyant greasy dirt and dust, use concentrated nitric acid oxidation again, make wooden ceramic powder surface form micropore or etching groove with organic solvent or tensio-active agent; Remove other impurity of surface, improve the binding ability of wooden ceramic powder and metal, then with the sensitization of the tin protochloride aqueous solution; Make wooden ceramic powder surface adsorption one deck that the metals ion of reductibility arranged, adopt colloidal pd activation solution that activation is carried out on wooden ceramic powder surface again, after the activation; Wood ceramics powder surface adsorption be to be the micelle of core with the atom palladium, can play katalysis for making palladium, need to be adsorbed on the Bivalent Tin colloid layer removal on every side of palladium atom; Promptly carry out dispergation and handle, dispergation can adopt concentrated hydrochloric acid solution or sodium acetate soln to handle at normal temperatures.Through above pre-treatment step, forming with the palladium atom on wooden ceramics powder surface is core autocatalysis center, makes its surface have the function of catching metals ion, could be at wooden ceramics powder coating surface layer of even metal level.
The wooden ceramics powder of conduction of the present invention is a kind of core-shell type matrix material of wooden ceramics powder/metal composite, and the wooden ceramics powder of metal and vesicular structure is compound can to absorb hertzian wave effectively, especially for wideband 100KHz～30000MHz absorption of electromagnetic wave.Can be as the conductive filler material that is used as the preparation electromagnetic shielding material; This conductive filler material is prone to homodisperse, can set up the favorable conductive network, and the vesicular structure of wood pottery can make hertzian wave portion's multiple reflection absorption within it again; Cause it to decay gradually; Thereby improve its shield effectiveness, can replace the high fillers of cost such as metal, graphite, carbon black, reduce the cost of conductive filler material greatly.Conducting electricity the metal level of wooden ceramics powder coating surface can be according to actual request for utilization, the sintering process of adjustment wood pottery, changes the plating amount of metal, manufactures and designs the conduction wood ceramics powder with certain electric magnetic shield performance in the wider frequency range thereby be implemented in.
The volume specific resistance of the wooden ceramics powder of conduction of the present invention is 4.5 * 10
-2Ω .cm～5.5 * 10
-1Ω .cm.Because of it is a powder body material; Can add according to the enforcement needs and with powder and prepare electrically conducting coating in the coating; Also can the bulk material that be pressed into different shape behind the powder body material binder mixture have been enlarged the range of application of electro-conductive material, can be used for using as electromagnetic shielding material.
Description of drawings
Fig. 1 is the stereoscan photograph of the conduction wood ceramics powder of test one preparation.
Embodiment
Embodiment one: the wooden ceramics powder of a kind of conduction of this embodiment is to be core body with wooden ceramics powder, and at the conductive powder body of core surface chemical plating layer of metal film, the adhesion amount of metal is 1%～50% of a wooden ceramics powder quality; Wherein metal is nickel, iron or cobalt.
The conduction wood ceramics powder of this embodiment is a kind of core-shell type matrix material of wooden ceramics powder/metal composite, and the wooden ceramics powder of metal and vesicular structure is compound can to absorb hertzian wave effectively, especially for wideband 100KHz～30000MHz absorption of electromagnetic wave.Can be as the conductive filler material that is used as the preparation electromagnetic shielding material; This conductive filler material is prone to homodisperse, can set up the favorable conductive network, and the vesicular structure of wood pottery can make hertzian wave portion's multiple reflection absorption within it again; Cause it to decay gradually; Thereby improve its shield effectiveness, can replace the high fillers of cost such as metal, graphite, carbon black, reduce the cost of conductive filler material greatly.Conducting electricity the metal level of wooden ceramics powder coating surface can be according to actual request for utilization, the sintering process of adjustment wood pottery, changes the plating amount of metal, manufactures and designs the conduction wood ceramics powder with certain electric magnetic shield performance in the wider frequency range thereby be implemented in.The volume specific resistance of the conduction wood ceramics powder of this embodiment is 4.5 * 10
-2Ω .cm～5.5 * 10
-1Ω .cm.Can be used for conductive filler material as electromagnetic shielding material.
Embodiment two: what this embodiment and embodiment one were different is: the adhesion amount of metal is 5%～40% of a wooden ceramics powder quality.Other is identical with embodiment one.
Embodiment three: what this embodiment was different with embodiment one or two is: the preparation method as the wooden ceramics powder of core body is undertaken by following: be to be dried to over dry under 30 ℃～100 ℃ the condition in temperature with biomass material; Then with the exsiccant biomass material under vacuum environment or protection of inert gas; At 600 ℃～2500 ℃ sintering 2h～10h of temperature; Be crushed to granularity 0.1 μ m～200 μ m with ball mill again, obtain wooden ceramics powder as core body; Wherein biomass material is timber, nut-shell, bamboo wood, rice husk, coffee grounds, tea grounds, tobacco rod, bagasse, xylogen or waste paper.Other is identical with embodiment one or two.
Embodiment four: what this embodiment was different with embodiment one or two is: the preparation method as the wooden ceramics powder of core body carries out according to the following steps: a, with biomass material be immersed in keep 20h～30h in the resin after; Biomass material is filtered out; And be that to be dried to water ratio under 30 ℃～100 ℃ the condition be 1%～3% in temperature, obtain dried particles; Again dried particles being placed on temperature is to keep 6h～10h in 180 ℃～220 ℃ the baking oven, obtains cured granulate; B, under vacuum environment or protection of inert gas, at 600 ℃～2500 ℃ sintering 2h～10h of temperature, using ball mill to be crushed to granularity again is 0.1 μ m～200 μ m, obtains the wooden ceramics powder as core body with the cured granulate of step a preparation; Wherein biomass material is timber, nut-shell, bamboo wood, rice husk, coffee grounds, tea grounds, tobacco rod, bagasse, xylogen or waste paper among the step a; Wherein the resin among the step a is resol, epoxy resin, urethane, polysulfone resin or polyimide resin.Other is identical with embodiment one or two.
Embodiment five: a kind of preparation method of conducting electricity wooden ceramics powder of this embodiment carries out according to the following steps:
One, join wooden ceramics powder in organic solvent or the tensio-active agent, ultra-sonic dispersion 10min～15min filters out wooden ceramics powder then, after deionized water wash, drying, obtains clean wooden ceramics powder;
It is to stir 10min～15min in 60%～65% the concentrated nitric acid solution that the wooden ceramics powder of the cleaning that two, step 1 is obtained joins mass percent concentration; Then wooden ceramics powder is filtered out; To neutrality, drying, obtain the wooden ceramics powder of surface oxidation with deionized water rinsing;
Three, being that 37% hydrochloric acid is solvent with mass percentage concentration, is that 10g/L is dissolved in tin protochloride in the hydrochloric acid solvent by the concentration of tin protochloride, obtains stannous chloride solution; The wooden ceramics powder of the surface oxidation that step 2 is obtained is added in the stannous chloride solution; Be to stir 30min～45min under 50 ℃～60 ℃ the condition in temperature; Then wooden ceramics powder is filtered out, after deionized water wash, drying, obtain sensitization wood ceramics powder;
Four, the sensitization wood ceramics powder that step 3 is obtained joins in the colloidal pd activation solution; Be to stir 20min～30min under 35 ℃～50 ℃ the condition in temperature, after wooden ceramics powder is filtered out, join in the hydrochloric acid soln; Be to stir 1min～3min under 40 ℃ the condition in temperature; Again wooden ceramics powder is filtered out, after deionized water wash, drying, obtain the wooden ceramics powder of surperficial pre-treatment;
The wooden ceramics powder of the surperficial pre-treatment that five, step 4 is obtained joins and keeps 40min～50min in the chemical plating fluid, then through filtering, after deionized water wash to neutral, the drying, obtaining conducting electricity wooden ceramics powder.
The conduction wood ceramics powder of this embodiment is a kind of core-shell type matrix material of wooden ceramics powder/metal composite, and the wooden ceramics powder of metal and vesicular structure is compound can to absorb hertzian wave effectively, especially for wideband 100KHz～30000MHz absorption of electromagnetic wave.Can be as the conductive filler material that is used as the preparation electromagnetic shielding material; This conductive filler material is prone to homodisperse, can set up the favorable conductive network, and the vesicular structure of wood pottery can make hertzian wave portion's multiple reflection absorption within it again; Cause it to decay gradually; Thereby improve its shield effectiveness, can replace the high fillers of cost such as metal, graphite, carbon black, reduce the cost of conductive filler material greatly.Conducting electricity the metal level of wooden ceramics powder coating surface can be according to actual request for utilization, the sintering process of adjustment wood pottery, changes the plating amount of metal, manufactures and designs the conduction wood ceramics powder with certain electric magnetic shield performance in the wider frequency range thereby be implemented in.The volume specific resistance of the conduction wood ceramics powder of this embodiment is 4.5 * 10
-2Ω .cm～5.5 * 10
-1Ω .cm.Can be used for conductive filler material as electromagnetic shielding material.
Embodiment six: this embodiment and embodiment five are different is that tensio-active agent in the step 1 is that anionic is or/and non-ionics.Other is identical with embodiment five.
Embodiment seven: this embodiment is different with embodiment five or six is that organic solvent in the step 1 is with acetone or methylethyl copper.Other is identical with embodiment five.
Embodiment eight: this embodiment is different with one of embodiment five to seven is that colloidal pd activation solution is that concentration by Palladous chloride is that the concentration of 1.0g/L, tin protochloride is that 70g/L, mass percent concentration are that the concentration of 37% hydrochloric acid be 300mL/L with Palladous chloride, tin protochloride and mass percent concentration is that 37% hydrochloric acid is added to the water formulated in the step 4.Other is identical with one of embodiment five to seven.
Embodiment nine: this embodiment is different with one of embodiment five to eight is that concentrated hydrochloric acid in the step 4 is that mass percent concentration is 37% concentrated hydrochloric acid.Other is identical with one of embodiment five to eight.
Embodiment ten: this embodiment is different with one of embodiment five to nine, and to be that chemical plating solution in the step 5 is that concentration by main salt is that the concentration of 35g/L～50g/L, sodium laurylsulfonate is that the concentration of 3g/L～5g/L, sodium hypophosphite is that the concentration of 70g/L～85g/L, Trisodium Citrate is that the concentration of 80g/L～100g/L, ammonium chloride is that the concentration of 100g/L～120g/L, lead sulfate is that 2mg/L～4mg/L is added to the water main salt, sodium laurylsulfonate, sodium hypophosphite, Trisodium Citrate, ammonium chloride and lead sulfate formulated, and wherein main salt is single nickel salt, ferric sulfate, rose vitriol, nickelous chloride, iron(ic)chloride or NSC 51149.Other is identical with one of embodiment five to nine.
The preferred chemical plating solution of this embodiment is that the concentration by main salt is that the concentration of 40g/L, sodium laurylsulfonate is that the concentration of 4g/L, sodium hypophosphite is that the concentration of 80g/L, Trisodium Citrate is that the concentration of 90g/L, ammonium chloride is that the concentration of 110g/L, lead sulfate is that 3mg/L is added to the water main salt, sodium laurylsulfonate, sodium hypophosphite, Trisodium Citrate, ammonium chloride and lead sulfate formulated.
The present invention is with following verification experimental verification beneficial effect of the present invention:
Test one: preparation is as the wooden ceramics powder of core body earlier; Its preparation method carries out according to the following steps: a, the sanding wood powder is crushed to below 80 orders; Wood powder does not need drying; Directly using solids content is the resin impregnating 40h of 30% (quality), and wherein solids content is that the liquid phenolic resin of 30% (quality) and the mass ratio of sanding wood powder are 0.2: 1, then the sanding wood powder is filtered out; Be placed on temperature and be in 80 ℃ the constant temperature air dry oven and be dried to water ratio＜3%, obtain the Procuring particle; Under 180 ℃, be dried to the resin completely solidified then, obtain cured granulate; B, be under the condition of 0.095MPa in vacuum tightness, with cured granulate sintering 6h under the condition of 900 ℃ of temperature of step a preparation, pulverize with ball mill again that wherein ball material mass ratio is 3: 1, the ball milling time is 60min, obtains the wooden ceramics powder as core body; Wherein the preparation method of the resol among the step a is following: take by weighing 100g phenol, the 162.5g mass percent concentration is 37% formaldehyde, and the 16.7g mass percent concentration is 42% sodium hydroxide; The phenol that melts is joined in the reaction kettle agitator, hydro-oxidation sodium solution; Under temperature is 50 ℃ condition, react 10min then, in 60min, join formaldehyde in the reaction kettle again and the temperature of controlling reaction solution at 65 ℃～80 ℃, add formaldehyde after; After reacting liquid temperature rises to 95 ℃; After the reaching viscosity and reach 35s (being coated with-4 glasss) of resin, cooling makes the temperature of resin in 100min, reduce to 30 ℃ from 95 ℃ rapidly; Obtain resol, its solids content is 30% (quality).
As the wooden ceramics powder of core body preparation conduction, the preparation method of wooden ceramics powder of conducting electricity carries out according to the following steps with the top wooden ceramics powder that obtains:
One, wooden ceramics powder joins in the acetone, and ultrasonic minute vibrating dispersion 10min filters out wooden ceramics powder then, with deionized water wash twice, is that 0.095MPa, temperature are vacuum-drying 12h under 80 ℃ the condition in vacuum tightness again, obtains clean wooden ceramics powder;
It is to stir 10min in 63% the concentrated nitric acid solution that the wooden ceramics powder of the cleaning that two, step 1 is obtained joins mass percent concentration; Then wooden ceramics powder is filtered out; Use deionized water wash to neutral, be vacuum-drying 12h under 80 ℃ the condition as 0.095MPa, temperature in vacuum tightness again, obtain the oxidized wooden ceramics powder in surface;
Three, be that 37% hydrochloric acid is solvent with mass percentage concentration; Concentration by tin protochloride is that 10g/L is dissolved in tin protochloride in the hydrochloric acid solvent; Obtain stannous chloride solution, the wooden ceramics powder with the surface oxidation of step 2 preparation joins in the tin protochloride aqueous solution then, in temperature is to stir 30min under 60 ℃ the condition; Then wooden ceramics powder is filtered out; To neutral, is 0.095MPa, temperature be 80 ℃ condition under vacuum-drying 12h in vacuum tightness again with deionized water wash, obtains sensitization wood ceramics powder;
Four, the sensitization wood ceramics powder that step 3 is obtained is distributed in the colloidal pd activation solution; In temperature is that 40 ℃ condition stirs 20min, after wooden ceramics powder is filtered out, joins mass percent concentration again and is in 37% the concentrated hydrochloric acid; Be to stir 1min under 40 ℃ the condition in temperature; Again wooden ceramics powder is filtered out, use deionized water wash to neutral, be vacuum-drying 12h under 80 ℃ the condition as 0.095MPa, temperature in vacuum tightness again, obtain the wooden ceramics powder of surperficial pre-treatment; Wherein colloidal pd activation solution is that the concentration by Palladous chloride is that the concentration of 1.0g/L, tin protochloride is that 70g/L, mass percent concentration are that the concentration of 37% hydrochloric acid be 300mL/L with Palladous chloride, tin protochloride and mass percent concentration is that 37% hydrochloric acid is added to the water formulated;
Five, be that the concentration of 35g/L, sodium hypophosphite is that the concentration of 70g/L, sodium laurylsulfonate is that the concentration of 3g/L, Trisodium Citrate is that the concentration of 20g/L, ammonium chloride is that the concentration of 120ml/L, lead sulfate is 2mg/L by the concentration of single nickel salt; The preparation chemical nickel-plating solution; The wooden ceramics powder of the surperficial pre-treatment that then step 4 is obtained joins in the chemical nickel-plating solution; Induction stirring 40min filters out wooden ceramics powder then, and is extremely neutral with deionized water wash; Be that 0.095MPa, temperature are vacuum-drying 12h under 80 ℃ the condition in vacuum tightness again, obtain conducting electricity wooden ceramics powder.
The conduction wood ceramics powder of this test one preparation is to be core body with wooden ceramics powder, and at the conductive powder body of core surface chemical plating layer of metal nickel, the adhesion amount of metallic nickel is 25% of a wooden ceramics powder quality.The stereoscan photograph of the conduction wood ceramics powder of this test one preparation is as shown in Figure 1, and Fig. 1 has shown the wooden ceramics powder configuration of surface after the nickel plating.This conducts electricity wooden ceramics powder at 40kg/cm
2Pressure under volume specific resistance be 8.4 * 10
-2Ω .cm.
Test two: preparation is as the wooden ceramics powder of core body earlier; Its preparation method carries out according to the following steps: a, walnut shell flour is crushed to below 80 orders; Walnut shell flour does not need drying, and directly using solids content is the resin impregnating 40h of 30% (quality), then walnut shell flour is filtered out from resol; Be placed on temperature and be in 60 ℃ the constant temperature air dry oven and be dried to water ratio＜3%, obtain the Procuring particle; And then to be placed on temperature be to be dried to the resin completely solidified in 180 ℃ the baking oven, obtains cured granulate; B, under nitrogen protection, with cured granulate sintering 6h under the condition of 800 ℃ of temperature of step a preparation, pulverize with ball mill again, wherein ball material mass ratio is 3: 1, the ball milling time is 60min, obtains the wooden ceramics powder as core body; Wherein the preparation method of the resol among the step a is following: take by weighing 100g phenol, the 162.5g mass percent concentration is 37% formaldehyde, and the 16.7g mass percent concentration is 42% sodium hydroxide; The phenol that melts is joined in the reaction kettle agitator, hydro-oxidation sodium solution; Under temperature is 45 ℃ condition, react 10min then, in 70min, join formaldehyde in the reaction kettle again and the temperature of controlling reaction solution at 65 ℃～80 ℃, add formaldehyde after; After reacting liquid temperature rises to 90 ℃; After the reaching viscosity and reach 32s (being coated with-4 glasss) of resin, cooling makes the temperature of resin in 120min, reduce to 30 ℃ from 90 ℃ rapidly; Obtain resol, its solids content is 30% (quality).
As the wooden ceramics powder of core body preparation conduction, the preparation method of wooden ceramics powder of conducting electricity carries out according to the following steps with the top wooden ceramics powder that obtains:
One, wooden ceramics powder joins ultra-sonic dispersion 10min in the acetone, then wooden ceramics powder is filtered out, and with deionized water wash twice, be that 0.095MPa, temperature are vacuum-drying 12h under 80 ℃ the condition in vacuum tightness again, obtain clean wooden ceramics powder;
It is to stir 10min in 63% the concentrated nitric acid solution that the wooden ceramics powder of the cleaning that two, step 1 is obtained joins mass percent concentration; Then wooden ceramics powder is filtered out; Use deionized water wash to neutral, be vacuum-drying 12h under 80 ℃ the condition as 0.095MPa, temperature in vacuum tightness again, obtain the oxidized wooden ceramics powder in surface;
Three, being that 37% hydrochloric acid is solvent with mass percentage concentration, is that 10g/L is dissolved in tin protochloride in the hydrochloric acid solvent by the concentration of tin protochloride, obtains stannous chloride solution; Wooden ceramics powder with the oxidation of step 2 preparation joins in the tin protochloride aqueous solution then; Be to stir 30min under 60 ℃ the condition in temperature; Then wooden ceramics powder is filtered out; To neutral, is 0.095MPa, temperature be 80 ℃ condition under vacuum-drying 12h in vacuum tightness again with deionized water wash, obtains sensitization wood ceramics powder;
Four, the sensitization wood ceramics powder that step 3 is obtained is distributed in the colloidal pd activation solution; In temperature is that 40 ℃ condition stirs 20min, after wooden ceramics powder is filtered out, joins mass percent concentration and is in 37% the concentrated hydrochloric acid; Be to stir 1min under 40 ℃ the condition in temperature; Again wooden ceramics powder is filtered out, use deionized water wash to neutral, be vacuum-drying 12h under 80 ℃ the condition as 0.095MPa, temperature in vacuum tightness again, obtain wooden ceramics powder through surperficial pre-treatment; Wherein colloidal pd activation solution is that the concentration by Palladous chloride is that the concentration of 1.0g/L, tin protochloride is that 70g/L, mass percent concentration are that the concentration of 37% hydrochloric acid be 300mL/L with Palladous chloride, tin protochloride and mass percent concentration is that 37% hydrochloric acid is added to the water formulated;
Five, be that the concentration of 20g/L, sodium hypophosphite is that the concentration of 20g/L, sodium laurylsulfonate 1g/L, Trisodium Citrate is that the concentration of 50g/L, ammonium chloride is 40g/L preparation chemical nickel-plating solution by the concentration of rose vitriol; The wooden ceramics powder of the surperficial pre-treatment of process that then step 4 is obtained joins in the electroless cobalt plating solution; Induction stirring 90min; Then wooden ceramics powder is filtered out; To neutral, is 0.095MPa, temperature be 80 ℃ condition under vacuum-drying 12h in vacuum tightness again with deionized water wash, obtains conducting electricity wooden ceramics powder.
The conduction wood ceramics powder of this test two preparation is to be core body with wooden ceramics powder, and at the conductive powder body of core surface chemical plating layer of metal cobalt, the adhesion amount of cobalt metal is 18% of a wooden ceramics powder quality.This conducts electricity wooden ceramics powder at 40kg/cm
2Pressure under volume specific resistance be 9.0 * 10
-2Ω .cm.
Claims (10)
1. wooden ceramics powder of conduction, the wooden ceramics powder that it is characterized in that conducting electricity is to be core body with wooden ceramics powder, at the conductive powder body of core surface chemical plating layer of metal film, the adhesion amount of metal is 1%～50% of a wooden ceramics powder quality; Wherein metal is nickel, iron or cobalt.
2. the wooden ceramics powder of a kind of conduction according to claim 1, the adhesion amount that it is characterized in that metal is 5%～40% of a wooden ceramics powder quality.
3. the wooden ceramics powder of a kind of conduction according to claim 1 and 2; It is characterized in that being undertaken by following: be to be dried to over dry under 30 ℃～100 ℃ the condition with biomass material in temperature as the preparation method of the wooden ceramics powder of core body; Then with the exsiccant biomass material under vacuum environment or protection of inert gas; At 600 ℃～2500 ℃ sintering 2h～10h of temperature, be crushed to granularity 0.1 μ m～200 μ m with ball mill again, obtain wooden ceramics powder as core body; Wherein biomass material is timber, nut-shell, bamboo wood, rice husk, coffee grounds, tea grounds, tobacco rod, bagasse, xylogen or waste paper.
4. the wooden ceramics powder of a kind of conduction according to claim 1 and 2; It is characterized in that carrying out according to the following steps as the preparation method of the wooden ceramics powder of core body: a, with biomass material be immersed in keep 20h～30h in the resin after; Biomass material is filtered out; And be that to be dried to water ratio under 30 ℃～100 ℃ the condition be 1%～3% in temperature, obtain dried particles; Again dried particles being placed on temperature is to keep 6h～10h in 180 ℃～220 ℃ the baking oven, obtains cured granulate; B, under vacuum environment or protection of inert gas, at 600 ℃～2500 ℃ sintering 2h～10h of temperature, using ball mill to be crushed to granularity again is 0.1 μ m～200 μ m, obtains the wooden ceramics powder as core body with the cured granulate of step a preparation; Wherein biomass material is timber, nut-shell, bamboo wood, rice husk, coffee grounds, tea grounds, tobacco rod, bagasse, xylogen or waste paper among the step a; Wherein the resin among the step a is resol, epoxy resin, urethane, polysulfone resin or polyimide resin.
5. a kind of preparation method of conducting electricity wooden ceramics powder as claimed in claim 1; The preparation method of wooden ceramics powder of it is characterized in that conducting electricity carries out according to the following steps: one, join wooden ceramics powder in organic solvent or the tensio-active agent; Ultra-sonic dispersion 10min～15min; Then wooden ceramics powder is filtered out, after deionized water wash, drying, obtain clean wooden ceramics powder; It is to stir 10min～15min in 60%～65% the concentrated nitric acid solution that the wooden ceramics powder of the cleaning that two, step 1 is obtained joins mass percent concentration; Then wooden ceramics powder is filtered out; To neutrality, drying, obtain the wooden ceramics powder of surface oxidation with deionized water rinsing; Three, being that 37% hydrochloric acid is solvent with mass percentage concentration, is that 10g/L is dissolved in tin protochloride in the hydrochloric acid solvent by the concentration of tin protochloride, obtains stannous chloride solution; The wooden ceramics powder of the surface oxidation that step 2 is obtained is added in the stannous chloride solution; Be to stir 30min～45min under 50 ℃～60 ℃ the condition in temperature; Then wooden ceramics powder is filtered out, after deionized water wash, drying, obtain sensitization wood ceramics powder; Four, the sensitization wood ceramics powder that step 3 is obtained joins in the colloidal pd activation solution; Be to stir 20min～30min under 35 ℃～50 ℃ the condition in temperature, after wooden ceramics powder is filtered out, join in the concentrated hydrochloric acid; Be to stir 1min～3min under 40 ℃ the condition in temperature; Again wooden ceramics powder is filtered out, after deionized water wash, drying, obtain the wooden ceramics powder of surperficial pre-treatment; The wooden ceramics powder of the surperficial pre-treatment that five, step 4 is obtained joins and keeps 40min～50min in the chemical plating fluid, then through filtering, after deionized water wash to neutral, the drying, obtaining conducting electricity wooden ceramics powder.
6. a kind of preparation method of conducting electricity wooden ceramics powder according to claim 5 is characterized in that the tensio-active agent in the step 1 is that anionic is or/and non-ionics.
7. according to claim 5 or 6 described a kind of preparing methods of conducting electricity wooden ceramics powder, it is characterized in that organic solvent in the step 1 is with acetone or methylethyl copper.
8. according to claim 5 or 6 described a kind of preparing methods of conducting electricity wooden ceramics powder, it is characterized in that colloidal pd activation solution in the step 4 is that concentration by Palladous chloride is that the concentration of 1.0g/L, tin protochloride is that 70g/L, mass percent concentration are that the concentration of 37% hydrochloric acid be 300mL/L with Palladous chloride, tin protochloride and mass percent concentration is that 37% hydrochloric acid is added to the water formulated.
9. according to claim 5 or 6 described a kind of preparing methods of conducting electricity wooden ceramics powder, it is characterized in that the concentrated hydrochloric acid in the step 4 is that mass percent concentration is 37% concentrated hydrochloric acid.
10. according to claim 5 or 6 described a kind of preparing methods of conducting electricity wooden ceramics powder; It is formulated to it is characterized in that chemical plating solution in the step 5 is that concentration by main salt is that the concentration of 35g/L～50g/L, sodium laurylsulfonate is that the concentration of 3g/L～5g/L, sodium hypophosphite is that the concentration of 70g/L～85g/L, Trisodium Citrate is that the concentration of 80g/L～100g/L, ammonium chloride is that the concentration of 100g/L～120g/L, lead sulfate is that 2mg/L～4mg/L is added to the water main salt, sodium laurylsulfonate, sodium hypophosphite, Trisodium Citrate, ammonium chloride and lead sulfate, and wherein main salt is single nickel salt, ferric sulfate, rose vitriol, nickelous chloride, iron(ic)chloride or NSC 51149.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105327578A (en) * | 2015-09-02 | 2016-02-17 | 中国科学院过程工程研究所 | Dusty gas purifying method |
| CN106520071A (en) * | 2016-12-06 | 2017-03-22 | 吉林大学 | Rice husk based C/magnetic Co particle composite wave absorber and preparation method thereof |
| CN113829686A (en) * | 2021-09-18 | 2021-12-24 | 安徽农业大学 | Degradable polymer-based biochar electromagnetic shielding composite material and preparation method thereof |
| CN114538568A (en) * | 2022-02-15 | 2022-05-27 | 河南省高新技术实业有限公司 | Ceramic catalytic electrode material for hybrid paper mulberry trees and preparation method and application thereof |
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| CN102107866A (en) * | 2010-12-15 | 2011-06-29 | 中国林业科学研究院木材工业研究所 | Method for preparing wood conductive carbon powder through high-temperature carbonization |
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| CN102107866A (en) * | 2010-12-15 | 2011-06-29 | 中国林业科学研究院木材工业研究所 | Method for preparing wood conductive carbon powder through high-temperature carbonization |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105327578A (en) * | 2015-09-02 | 2016-02-17 | 中国科学院过程工程研究所 | Dusty gas purifying method |
| CN106520071A (en) * | 2016-12-06 | 2017-03-22 | 吉林大学 | Rice husk based C/magnetic Co particle composite wave absorber and preparation method thereof |
| CN106520071B (en) * | 2016-12-06 | 2018-05-25 | 吉林大学 | Rice husk base carbon/magnetism Co particle composite wave-absorbing agent and preparation method thereof |
| CN113829686A (en) * | 2021-09-18 | 2021-12-24 | 安徽农业大学 | Degradable polymer-based biochar electromagnetic shielding composite material and preparation method thereof |
| CN114538568A (en) * | 2022-02-15 | 2022-05-27 | 河南省高新技术实业有限公司 | Ceramic catalytic electrode material for hybrid paper mulberry trees and preparation method and application thereof |
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