CN102864322B - Method for preparing high-porosity material by formed knitting technology - Google Patents
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- CN102864322B CN102864322B CN201210332338.8A CN201210332338A CN102864322B CN 102864322 B CN102864322 B CN 102864322B CN 201210332338 A CN201210332338 A CN 201210332338A CN 102864322 B CN102864322 B CN 102864322B
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Abstract
The invention discloses a method for preparing the high-porosity material by the formed knitting technology. The formed knitting technology is adopted, a three-dimensional organic template is dipped and coated by taking a polyester filament as raw material; then high-temperature oxidation reaction is carried out by secondary dipping; finally, decomposing metallic oxide under the high vacuum condition of 900DEG C; and sintering at the temperature of 950DEG C so as to successfully prepare foamy copper with a high-porosity tapping structure. The method disclosed by the invention is simple and easy to realize. The prepared high-porosity foamy copper combines the performances of low density, high rigidity, impact performance, sound attenuation, noise reduction, electromagnetic shielding, ventilation, water permeability, low heat conductivity and the like, has a good damping characteristic and can be widely applied to industries, such as aerospace, aviation, atomic energy, environment protection and electrochemistry.
Description
Technical field
The invention belongs to technical field of material, relate to a kind of preparation method of high porosity material, be specifically related to a kind of method that adopts shaping knitting technology to prepare high porosity material.
Background technology
High porosity metal material is a kind of new engineering material that has function and structure double attribute concurrently that recent two decades develops rapidly in the world.Performances such as this material combines low density, high rigidity, impacts energy absorption capacity, dry, electromagnetic shielding falls in noise reduction, air-and water-permeable, lower thermal conductivity and have good damping characteristic, are therefore widely used in the industries such as space flight, aviation, nuclear power, environmental protection and electrochemistry.
The preparation method of high porosity metal material mainly comprises casting, foaming, deposition, sintering etc.From investigative technique, wide aperture (cm) foamed metal solid netted and small-bore (μ m), low density high voidage is the emphasis of breaking through in current technology of preparing.Many scholars both domestic and external have done the work differing from one another in this regard.Yet all there is complex process in these methods, the shortcoming such as high, the selectable material of cost is restricted.
Shaping knitting technology is the Yi Ge branch that in knitting industry in nearly ten years, fast development is got up.It has overturned traditional knitting process, can participate in the pin number of braiding and the size and dimension that line number changes fabric by change.It is a kind of quite promising method of the three-dimensional organic formwork of preparation high porosity foam material.At present, in the research of the relevant this respect of foamed metal preparation field, report also seldom.
Summary of the invention
The object of this invention is to provide a kind of method that adopts shaping knitting technology to prepare high porosity material, preparation method's complexity, template forming technical sophistication of existing high porosity metal material, the problem that cost of goods manifactured is high have been solved, the method makes full use of the advantage of shaping knitting technology braiding three-dimensional template, and preparation method is easy.Meanwhile, the method can reduce cost of goods manifactured and saving resource again, for multidisciplinary crossbar system provides good thinking and method for functional materials.
The technical solution adopted in the present invention is, a kind of method that adopts shaping knitting technology to prepare high porosity material is specifically implemented according to following steps:
Step 1: prepare the three-dimensional organic formwork of high porosity;
Step 2: the three-dimensional organic formwork that step 1 is obtained carries out pre-treatment;
Step 3: prepare metal paste;
Step 4: single-steeping: the pretreated three-dimensional organic formwork that step 2 is obtained impregnated in the metal paste that step 3 obtains after 40min-60min, with fluidizing air, remove unnecessary slurry, room temperature blowing down blower fan blows 15min-20min, forms porous three-dimensional biscuit after 60 ℃ of dry 15min-20min;
Step 5: double-steeping: repeating step 4, drying conditions is changed to 60 ℃, and 20min-30min obtains the porous three-dimensional biscuit after double-steeping;
Step 6: decompose organic formwork: the porous three-dimensional biscuit obtaining in step 5 is decomposed to terylene under oxidizing condition, 400 ℃ of temperature, 20min-30min, obtains porous copper oxide;
Step 7: vacuum sintering foam copper: by the porous copper oxide obtaining in step 6 in room temperature-900 ℃, 4.5 * 10
-2-5 * 10
-2under Pa vacuum condition, make metal oxide decompose, and carry out sintering under 900 ℃ of-950 ℃ of conditions, obtain the foam copper of three-dimensional netted through hole.
Feature of the present invention is also,
Step 1 is wherein prepared the three-dimensional organic formwork of high porosity, specifically according to following steps, implement: on the hand knitting machine of 5 plane No., with polyester filament, as raw material, form braiding, front and back needle-bar is first pressed 1+1 rib starting, by a line of the common braiding of front and back needle-bar, then before and after adjusting successively, the raising cam of needle-bar, weaves by the method for round shape braiding, obtains the three dimensional fabric that base and two ends are all sealed, centre is empty tube shape; The terylene adopting is 150D/36F, when fiber is made, uses spinning jet, conventional 150D, and spinning jet has 36 holes.
The three-dimensional organic formwork that step 2 wherein pair step 1 obtains carries out pre-treatment, specifically according to following steps, implements: adopt the NaOH solution of 1mol/L, at 60 ℃ of-90 ℃ of temperature, soak 120min-150nin.
Metal paste in step 3 wherein, composed of the following components according to mass percent: the copper powder of 3%-5%, the polyvinyl alcohol of 10%-15%, the methylcellulose gum of 5%-7%, the tensio-active agent of 3%-5%, the ammoniacal liquor of 5%-7%, surplus is water, the mass percent sum of above component is 100%, described copper powder, mean particle size is 400-1000 order, and powder particle is sheet, and average loose density is 1.2g/cm
3.
Tensio-active agent wherein adopts OP-10.
The invention has the beneficial effects as follows, the inventive method is simple, the performances such as prepared high porosity foam copper combines low density, high rigidity, impacts energy absorption capacity, dry, electromagnetic shielding falls in noise reduction, air-and water-permeable, lower thermal conductivity, and there is good damping characteristic.Can be widely used in the industries such as space flight, aviation, nuclear power, environmental protection and electrochemistry.
Accompanying drawing explanation
Fig. 1 is that the present invention adopts shaping knitting technology to prepare the method process flow sheet of high porosity material;
Fig. 2 is three-dimensional organic formwork weave diagram and coil structure in the inventive method;
Fig. 3 is the relation curve of metal paste viscosity and pH value in the inventive method;
Fig. 4 is the XRD figure spectrum of the high porosity foam copper prepared of the inventive method;
Fig. 5 is foam copper pattern after an infiltration sintering in the inventive method;
Fig. 6 is foam copper pattern after secondary infiltration sintering in the inventive method;
Fig. 7 is high porosity foam copper stress under compression strain curve prepared by the inventive method.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
The present invention adopts shaping knitting technology to prepare the method for high porosity material, as shown in Figure 1, the terylene (PET) of take knits out the organic formwork of high porosity as raw material adopts shaping knitting technology, to preparing the foam copper of high porosity (﹥ 80%), open-celled structure after organic formwork infiltration.After secondary infiltration, foam copper material porosity change is little, and its stress plateau can be brought up to 1MPa from 0.5MPa, can be widely used in the industries such as aerospace, environmental protection and electrochemistry.Specifically according to following steps, implement:
Step 1: the preparation of the three-dimensional organic formwork of high porosity: as shown in Figure 2, " 0 " is initial line to the weave diagram of organic formwork.On the flying tiger participants in a bridge game operated knitting machine for knitting of 5 plane No., with polyester filament, as raw material, form braiding.Front and back needle-bar is first pressed 1+1 rib starting, by a line of the common braiding of forward and backward needle-bar, and the raising cam of needle-bar before and after then adjusting successively, the method weaving by round shape weaves.Can obtain base and two ends are all sealed, centre is the three dimensional fabric just as pocket of empty tube shape; The terylene adopting is 150D/36F.D(Denier, DENIER), the fineness unit of man-made fiber, the weight of 9000 meters of long man-made fiber (gram).When fiber is made, use spinning jet, conventional 150D, spinning jet has 36 holes.Be mass of fibers, by 36, form.Expression formula: 150D/36F.
Step 2: three-dimensional organic formwork pre-treatment: utilize the acidproof not alkaline-resisting characteristic of polyester material, adopt the NaOH solution of 1mol/L to carry out pre-treatment to it.At 60 ℃ of-90 ℃ of temperature, soak 120min-150nin.To increase fiber surface roughness, improve wettability and adhesivity between three-dimensional organic formwork and aqueous slurries;
Step 3: the preparation of metal paste: the component of metal paste is composed of the following components according to mass percent: the copper powder of 3%-5%, the polyvinyl alcohol of 10%-15%, the methylcellulose gum of 5%-7%, tensio-active agent (the OP-10 of 3%-5%, non-ionic type), the ammoniacal liquor of 5%-7%, surplus is water, the mass percent sum of above component is 100%.Wherein polyvinyl alcohol, methylcellulose gum are made respectively binding agent and dispersion agent, and tensio-active agent and ammoniacal liquor are for improving the rheological characteristics of slurry; The copper powder adopting is from glass station, Xi'an, and mean particle size is 400-1000 order, and powder particle is sheet, average loose density 1.2g/cm
3.Can the rheological of metal paste be prepare one of key factor of well behaved foam copper, provided the relation of slurry viscosity and pH value at rotating speed one timing (5r/min) Fig. 3.As can be seen from Figure 3, pH value is that the viscosity of 9.5 o'clock slurries is minimum, and mobility is best.
Step 4: single-steeping: the pretreated three-dimensional organic formwork that step 2 is obtained impregnated in the metal paste that step 3 obtains after 40min-60min, with fluidizing air, remove unnecessary slurry (room temperature blowing down blower fan blows 15min-20min), drying (60 ℃, 15min-20min) the rear porous three-dimensional biscuit that forms; Fig. 5 is foam copper pattern after an infiltration sintering, and the pore structure that as can be seen from the figure an infiltration sintering obtains is more sparse.
Step 5: double-steeping: repeating step 4, drying conditions is changed to 60 ℃, and 20min-30min obtains the porous three-dimensional biscuit after double-steeping; Fig. 6 is foam copper pattern after secondary infiltration sintering, and the pore structure that as can be seen from the figure secondary infiltration sintering obtains is dense.
Step 6: decompose organic formwork: the porous three-dimensional biscuit obtaining in step 5 is decomposed to terylene under oxidizing condition, and (400 ℃, 20min-30min), obtain porous copper oxide;
Step 7: vacuum sintering foam copper: by the porous copper oxide obtaining in step 6 under ℃ high-temperature vacuum condition of room temperature-900 (4.5 * 10
-2-5 * 10
-2pa) make metal oxide decompose and carry out sintering at 900 ℃-950 ℃, obtain the foam copper of three-dimensional netted through hole.As shown in Figure 7, the densification strain of the foam copper that once infiltration and secondary infiltration obtain is respectively 73.29% and 60.02% to high porosity foam copper stress under compression strain curve.Fig. 4 is the XRD figure spectrum of high porosity foam copper.
Embodiment 1
1) preparation of the three-dimensional organic formwork of high porosity: on the flying tiger participants in a bridge game operated knitting machine for knitting of 5 plane No., form braiding with polyester filament (150D/36F) as raw material.Front and back needle-bar is first pressed 1+1 rib starting, by a line of the common braiding of forward and backward needle-bar, and the raising cam of needle-bar before and after then adjusting successively, the method weaving by round shape weaves.Can obtain base and two ends are all sealed, centre is the three dimensional fabric just as pocket of empty tube shape;
2) three-dimensional organic formwork pre-treatment: utilize the acidproof not alkaline-resisting characteristic of polyester material, adopt the NaOH solution of 1mol/L to processing before.To increase fiber surface roughness, improve wettability and adhesivity between three-dimensional organic formwork and aqueous slurries;
3) preparation of metal paste: the composition of metal paste comprises copper powder (3%), water, polyvinyl alcohol (10%), methylcellulose gum (5%), tensio-active agent (3%) and ammoniacal liquor (5%).Wherein polyvinyl alcohol, methylcellulose gum are made respectively binding agent and dispersion agent, and tensio-active agent and ammoniacal liquor are for improving the rheological characteristics of slurry;
4) single-steeping: pretreated three-dimensional organic formwork in step 2 be impregnated in step 3 in the metal paste of preparation after 1h, with fluidizing air, remove unnecessary slurry (room temperature blowing down blower fan blows 20min), drying (60 ℃, 20min) the rear porous three-dimensional biscuit that forms;
5) double-steeping: repeating step 4, drying conditions is changed to 60 ℃, 30min;
6) decompose organic formwork: the porous three-dimensional biscuit obtaining in step 5 is decomposed to terylene under oxidizing condition, and (400 ℃, 30min), obtain porous copper oxide;
7) vacuum sintering foam copper: by the porous copper oxide foams that obtain in step 6 under 900 ℃ of high vacuum conditions (5 * 10
-2pa) make metal oxide decompose and carry out sintering at 950 ℃, obtain the foam copper of three-dimensional netted through hole.
Embodiment 2
1) preparation of the three-dimensional organic formwork of high porosity: on the flying tiger participants in a bridge game operated knitting machine for knitting of 5 plane No., form braiding with polyester filament (150D/48F) as raw material.Front and back needle-bar is first pressed 1+1 rib starting, by a line of the common braiding of forward and backward needle-bar, and the raising cam of needle-bar before and after then adjusting successively, the method weaving by round shape weaves.Can obtain base and two ends are all sealed, centre is the three dimensional fabric just as pocket of empty tube shape;
2) three-dimensional organic formwork pre-treatment: utilize the acidproof not alkaline-resisting characteristic of polyester material, adopt the NaOH solution of 0.8mol/L to processing before.To increase fiber surface roughness, improve wettability and adhesivity between three-dimensional organic formwork and aqueous slurries;
3) preparation of metal paste: the composition of metal paste comprises copper powder (5%), water, polyvinyl alcohol (15%), methylcellulose gum (7%), tensio-active agent (4%) and ammoniacal liquor (6%).Wherein polyvinyl alcohol, methylcellulose gum are made respectively binding agent and dispersion agent, and tensio-active agent and ammoniacal liquor are for improving the rheological characteristics of slurry;
4) single-steeping: pretreated three-dimensional organic formwork in step 2 be impregnated in step 3 in the metal paste of preparation after 2h, with fluidizing air, remove unnecessary slurry (room temperature blowing down blower fan blows 20min), drying (50 ℃, 30min) the rear porous three-dimensional biscuit that forms;
5) double-steeping: repeating step 4, drying conditions is changed to 50 ℃, 1h;
6) decompose organic formwork: the porous three-dimensional biscuit obtaining in step 5 is decomposed to terylene under oxidizing condition, and (350 ℃, 30min), obtain porous copper oxide;
7) vacuum sintering foam copper: by the porous copper oxide foams that obtain in step 6 under 900 ℃ of high vacuum conditions (5 * 10
-2pa) make metal oxide decompose and carry out sintering at 900 ℃, obtain the foam copper of three-dimensional netted through hole.
Embodiment 3
1) preparation of the three-dimensional organic formwork of high porosity: on the flying tiger participants in a bridge game operated knitting machine for knitting of 5 plane No., form braiding with polyester filament (150D/36F) as raw material.Front and back needle-bar is first pressed 1+1 rib starting, by a line of the common braiding of forward and backward needle-bar, and the raising cam of needle-bar before and after then adjusting successively, the method weaving by round shape weaves.Can obtain base and two ends are all sealed, centre is the three dimensional fabric just as pocket of empty tube shape;
2) three-dimensional organic formwork pre-treatment: utilize the acidproof not alkaline-resisting characteristic of polyester material, adopt the NaOH solution of 0.8mol/L to processing before.To increase fiber surface roughness, improve wettability and adhesivity between three-dimensional organic formwork and aqueous slurries;
3) preparation of metal paste: the composition of metal paste comprises copper powder (4%), water, polyvinyl alcohol (10%), methylcellulose gum (7%), tensio-active agent (5%) and ammoniacal liquor (5%).Wherein polyvinyl alcohol, methylcellulose gum are made respectively binding agent and dispersion agent, and tensio-active agent and ammoniacal liquor are for improving the rheological characteristics of slurry;
4) single-steeping: pretreated three-dimensional organic formwork in step 2 be impregnated in step 3 in the metal paste of preparation after 1h, with fluidizing air, remove unnecessary slurry (room temperature blowing down blower fan blows 20min), drying (60 ℃, 30min) the rear porous three-dimensional biscuit that forms;
5) double-steeping: repeating step 4, drying conditions is changed to 60 ℃, 40min;
6) decompose organic formwork: the porous three-dimensional biscuit obtaining in step 5 is decomposed to terylene under oxidizing condition, and (400 ℃, 30min), obtain porous copper oxide;
7) vacuum sintering foam copper: by the porous copper oxide foams that obtain in step 6 under 950 ℃ of high vacuum conditions (5 * 10
-2pa) make metal oxide decompose and carry out sintering at 950 ℃, obtain the foam copper of three-dimensional netted through hole.
Embodiment 4
1) preparation of the three-dimensional organic formwork of high porosity: on the flying tiger participants in a bridge game operated knitting machine for knitting of 5 plane No., form braiding with polyester filament (150D/36F) as raw material.Front and back needle-bar is first pressed 1+1 rib starting, by a line of the common braiding of forward and backward needle-bar, and the raising cam of needle-bar before and after then adjusting successively, the method weaving by round shape weaves.Can obtain base and two ends are all sealed, centre is the three dimensional fabric just as pocket of empty tube shape;
2) three-dimensional organic formwork pre-treatment: utilize the acidproof not alkaline-resisting characteristic of polyester material, adopt the NaOH solution of 1.2mol/L to processing before.To increase fiber surface roughness, improve wettability and adhesivity between three-dimensional organic formwork and aqueous slurries;
3) preparation of metal paste: the composition of metal paste comprises copper powder (3%), water, polyvinyl alcohol (10%), methylcellulose gum (7%), tensio-active agent (4%) and ammoniacal liquor (6%).Wherein polyvinyl alcohol, methylcellulose gum are made respectively binding agent and dispersion agent, and tensio-active agent and ammoniacal liquor are for improving the rheological characteristics of slurry;
4) single-steeping: pretreated three-dimensional organic formwork in step 2 be impregnated in step 3 in the metal paste of preparation after 30min, with fluidizing air, remove unnecessary slurry (room temperature blowing down blower fan blows 20min), drying (50 ℃, 30min) the rear porous three-dimensional biscuit that forms;
5) double-steeping: repeating step 4, drying conditions is changed to 50 ℃, 1h;
6) decompose organic formwork: the porous three-dimensional biscuit obtaining in step 5 is decomposed to terylene under oxidizing condition, and (450 ℃, 30min), obtain porous copper oxide;
7) vacuum sintering foam copper: by the porous copper oxide foams that obtain in step 6 under 900 ℃ of high vacuum conditions (5 * 10
-2pa) make metal oxide decompose and carry out sintering at 950 ℃, obtain the foam copper of three-dimensional netted through hole.
From principle aspect, inventive point of the present invention is described below:
1, select loop construction evenly, the three-dimensional polyester piece good of high opening rate does mould material, and adopts the NaOH solution of 1mol/L to processing before.To increase fiber surface roughness, improve wettability and adhesivity between three-dimensional organic formwork and aqueous slurries.This is mainly that acid resistance is greater than alkali resistance because terylene is polyester man-made fiber.The NaOH of 1mol/L, at 60 ℃ of-90 ℃ of temperature, soaks 120min-150min, is both effectively located in and has managed fiber surface, is unlikely to again to destroy internal structure and the physical index of fiber.Excess Temperature overlong time, can have excessive damage to fiber; The too low time of temperature is shorter, inadequate to the pre-treatment degree of fiber, can affect follow-up preparation.
2, can the quality of metal paste performance be prepare one of key factor of well behaved foam copper, and metal paste should have certain mobility and good thixotropy.The mobility of slurry is to guarantee to be evenly coated in the coil of many spaces organic precursor and the principal element on hole wall in slurry steeping process; The thixotropy of slurry can guarantee to keep in removing the process of unnecessary slurry presoma vesicular structure, avoid the generation of plug-hole defect.The composition of metal paste comprises copper powder, water, polyvinyl alcohol, methylcellulose gum, tensio-active agent and ammoniacal liquor.Wherein polyvinyl alcohol, methylcellulose gum are made respectively binding agent and dispersion agent, and tensio-active agent and ammoniacal liquor are for improving the rheological characteristics of slurry.The proportioning of pulp components of the present invention is optimum range, the too high or too low rheological property that all can affect slurry of each component proportion.
3, foam copper calcining system mainly comprises three phases: polyester (PET) catabolic phase (room temperature-350 ℃, air), cupric oxide catabolic phase (room temperature-900 ℃, vacuum tightness 5 * 10
-2pa) and the foam copper sintering stage (900 ℃-950 ℃, vacuum tightness 13Pa).Polyester decomposition course mainly occurs in the first stage, should control heating rate.Too fast if heated up, can cause porous insert to cave in, ftracture because organism vigorous oxidation produces a large amount of gas.The object of subordinate phase is under high vacuum condition (4.5 * 10
-2-5 * 10
-2pa) cupric oxide base substrate is resolved into the slightly porous foam copper of intensity.In this stage, should control heating rate and soaking time, in order to avoid cause base substrate to cave in and metal excessively volatilizees.Phase III is the sintering stage of Porous Cu, and cupric oxide can cause more room in resolving into the process of copper, and structure is comparatively loose, now should improve sintering temperature, and acceleration of sintering neck length, to improve foamy body, is controlled soaking time to reduce copper volatilization simultaneously.
Claims (3)
1. adopt shaping knitting technology to prepare a method for high porosity material, it is characterized in that, specifically according to following steps, implement:
Step 1: prepare the three-dimensional organic formwork of high porosity; Specifically according to following steps, implement: on the hand knitting machine of 5 plane No., with polyester filament, as raw material, form braiding, front and back needle-bar is first pressed 1+1 rib starting, by a line of the common braiding of front and back needle-bar, then the raising cam of needle-bar before and after adjusting successively, method by round shape braiding weaves, and obtains the three dimensional fabric that base and two ends are all sealed, centre is empty tube shape; The terylene adopting is 150D/36F, when fiber is made, uses spinning jet, conventional 150D, and spinning jet has 36 holes;
Step 2: the three-dimensional organic formwork that step 1 is obtained carries out pre-treatment;
Step 3: prepare metal paste; Described metal paste, composed of the following components according to mass percent: the copper powder of 3%-5%, the polyvinyl alcohol of 10%-15%, the methylcellulose gum of 5%-7%, the tensio-active agent of 3%-5%, the ammoniacal liquor of 5%-7%, surplus is water, the mass percent sum of above component is 100%, described copper powder, mean particle size is 400-1000 order, and powder particle is sheet, and average loose density is 1.2g/cm
3;
Step 4: single-steeping: the pretreated three-dimensional organic formwork that step 2 is obtained impregnated in the metal paste that step 3 obtains after 40min-60min, with fluidizing air, remove unnecessary slurry, room temperature blowing down blower fan blows 15min-20min, forms porous three-dimensional biscuit after 60 ℃ of dry 15min-20min;
Step 5: double-steeping: repeating step 4, drying conditions is changed to 60 ℃, and 20min-30min obtains the porous three-dimensional biscuit after double-steeping;
Step 6: decompose organic formwork: the porous three-dimensional biscuit obtaining in step 5 is decomposed to terylene under oxidizing condition, 400 ℃ of temperature, 20min-30min, obtains porous copper oxide;
Step 7: vacuum sintering foam copper: by the porous copper oxide obtaining in step 6 at 900 ℃, 4.5 * 10
-2-5 * 10
-2under Pa vacuum condition, make metal oxide decompose, and carry out sintering under 900 ℃ of-950 ℃ of conditions, obtain the foam copper of three-dimensional netted through hole.
2. employing shaping knitting technology according to claim 1 is prepared the method for high porosity material, it is characterized in that, the three-dimensional organic formwork that described step 2 pair step 1 obtains carries out pre-treatment, specifically according to following steps, implement: the NaOH solution that adopts 1mol/L, at 60 ℃ of-90 ℃ of temperature, soak 120min-150min.
3. employing shaping knitting technology according to claim 1 is prepared the method for high porosity material, it is characterized in that, described tensio-active agent adopts OP-10.
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| CN104451235B (en) * | 2014-12-15 | 2016-11-02 | 中国矿业大学 | A kind of method utilizing cupric oxide powder to prepare complicated shape Porous Cu |
| CN112692287B (en) * | 2021-01-14 | 2023-03-28 | 昆明理工大学 | Preparation method of ordered porous titanium in three-dimensional communicated latticed distribution |
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