CN103789548B - For the thermite of hypergravity aid burning synthesis Cu-base composites - Google Patents
For the thermite of hypergravity aid burning synthesis Cu-base composites Download PDFInfo
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Abstract
The invention belongs to conbustion synthesis and prepare technical field, be specifically related to the thermite for hypergravity aid burning synthesis Cu-base composites.Thermite of the present invention, the Al powder of the CuO powder adopting granular gradient to distribute in formula and granular gradient distribution, by adding Cu
2o powder, Cu powder, MgO powder and CaF
2the rate of combustion of reaction when Cu-base composites is prepared in powder regulation and control and thermal discharge, achieve stablizing of thermite reaction in super gravity field controlled.Thermite of the present invention has low splash rate, high thermal discharge, stablizes controlled feature, is applicable to the multiple Cu-base composites of hypergravity aid burning synthesis preparation.
Description
Technical field
The invention belongs to conbustion synthesis and prepare technical field, be specifically related to the thermite for hypergravity aid burning synthesis Cu-base composites.
Background technology
Cu-base composites can give full play to the characteristic such as high strength, high rigidity, low thermal coefficient of expansion of the high connductivity of matrix Cu, high thermal conduction characteristic and wild phase or composite bed, has excellent comprehensive physical performance and mechanical property.According to the feature of compound, Cu-base composites can be divided into granule enhancement type, fiber reinforcement type and plane to cover copper type three types.Particulates reinforcements in common granule enhancement type comprises W, Al
2o
3, SiC, AlN, diamond etc., the fiber reinforcement in fiber reinforcement type then comprises fiber C, fiber B, SiC fiber, tungsten filament etc. mutually.The Cu-base composites of different wild phase strengthening has been widely used in Electronic Packaging heat sink material, electrical contact material, resistance welding electrode, combustion liner, nuclear fusion stack towards plasma material etc.Powder metallurgic method, machine-alloying and infiltration method prepare the modal method of Cu-base composites, and various preparation method differs from one another in the regulation and control of Cu-base composites structure properties and cost control.Along with the continuous innovation of each art, while controlling cost, the performance of Cu-base composites is had higher requirement.The proposition of new preparation technology is applied widely provide possibility for being realized Cu-base composites.
Conbustion synthesis is that the chemical system of high heat release provides certain energy to bring out locally chemical reaction to occur by extraneous, form combustion reactions forward position, then self liberated heat of reaction is utilized to make combustion wave continuous spontaneous expanded forward in reaction system, till reactant is complete, thus synthesize the process of required material in a short period of time.Combustion synthesis process has the features such as energy utilization rate is high, temperature of combustion is high, combustionvelocity is fast, product is high-purity, instrument and supplies process is simple.At present, combustion synthesis process has been successfully applied to the preparation of multiple stupalith, metal matrix and ceramic matric composite, intermetallic compound, Functionally Graded Materials etc.But, combustion synthesis process due to speed of response fast, in building-up process, thermograde is large, and reaction controllability is poor, causes the porosity of product higher, is difficult to obtain purer metal or ceramic product.Special in preparing high-compactness metal matrix or ceramic matric composite, it is realize metal to be separated with ceramic phase and the best way of densification that outfield is assisted.Centrifugal force outfield is combined with combustion synthesis process the ceramic-lined and stainless steel lined composite steel tube prepared on a large scale commercial application in the conveying of aluminium liquid, geothermal water, oil and natural gas etc.But the auxiliary of common centrifugal force outfield (gravity coefficient is 150 ~ 200g) is also not enough to the preparation realizing high-compactness, high purity, the regulatable Cu-base composites of Structure and Properties.
The aid burning synthesis of hypergravity outfield utilizes thermite reaction to produce ultrahigh-temperature, the can ceramic product that reaction is generated is in molten state, impose hypergravity outfield (gravity coefficient is 500 ~ 10000g) simultaneously and realize being separated completely and densification of metal and ceramic droplet, hypergravity outfield to the strengthening of mass transfer and heat transfer process for realize the further structure regulating of material and performance boost provide very big may.When adopting the preparation of hypergravity aid burning synthesis technique to have the Cu-base composites of excellent combination physicals and mechanical property, suitable thermite system is selected to prepare matrix Cu of crucial importance.Common thermite reaction system, as Al-CuO system and CaSi
2-CuO system, has different rate of combustion and temperature of combustion, is mainly used in welding, is difficult to the needs meeting hypergravity aid burning synthesis technique in reaction stability, rate of combustion and temperature adjustable, product purity etc.Therefore, develop a kind of thermite system being applicable to hypergravity aid burning synthesis technique, seem particularly crucial.
Summary of the invention
The object of this invention is to provide a kind of for the hypergravity aid burning synthesis stable reaction of Cu-base composites, rate of combustion and temperature of combustion controllable, thermite that product purity is high; The thermite provided can realize the preparation of multiple Cu-base composites by hypergravity aid burning synthesis technique.
Technical conceive of the present invention is: for meeting the needs of hypergravity aid burning synthesis technique, and thermite need improve around following 3.One, the splash degree of thermite reaction is reduced; Two, the purity of thermite reaction product is improved; Three, the density of thermite reaction product is improved.The rate of combustion of thermite reaction and temperature of combustion are the keys regulating splash degree and density, and the use of additives in raw materials is then particularly important to the purity controlling product.
Of the present invention for the CuO powder that mainly distributed by granular gradient of thermite of hypergravity aid burning synthesis Cu-base composites and the Al powder of granular gradient distribution, and the Cu added
2o powder, MgO powder and CaF
2obtain after powder mixing.The Cu added
2o powder, MgO powder and CaF
2powder additives is used for the rate of combustion of thermite reaction, temperature of combustion and product purity.
The granular gradient of the CuO powder of described granular gradient distribution is distributed as 24 order > granularity >=100 orders, 100 order > granularity >=200 orders, 200 order > granularity >=300 orders.
The granular gradient of the Al powder of described granular gradient distribution is distributed as 30 order > granularity >=60 orders, 60 order > granularity >=100 orders, 100 order > granularity >=200 orders.
In thermite of the present invention, with the weight part of the CuO powder of described granular gradient distribution for benchmark, the CuO powder of the granular gradient distribution in described thermite is 35 ~ 75 weight parts, and the Al powder of granular gradient distribution is 8 ~ 12 weight parts, Cu
2o powder is 2 ~ 6 weight parts, and MgO powder is 5 ~ 10 weight parts, CaF
2powder is 1 ~ 6 weight part.
Wherein: it is 2 ~ 40 weight parts that the granular gradient in the CuO powder of described granular gradient distribution is distributed as 24 order > granularity >=100 object CuO powders, 100 order > granularity >=200 object CuO powders are 3 ~ 30 weight parts, and 200 order > granularity >=300 object CuO powders are 5 ~ 30 weight parts.
Wherein: it is 2 ~ 8 weight parts that the granular gradient in the Al powder of described granular gradient distribution is distributed as 30 order > granularity >=60 object Al powders, 60 order > granularity >=100 object Al powders are 2 ~ 4 weight parts, and 100 order > granularity >=200 object Al powders are 2 ~ 4 weight parts.
Further containing Cu powder in thermite of the present invention, with the weight part of the CuO powder of the granular gradient distribution described in described thermite for benchmark, the content of described Cu powder in described thermite is 0 ~ 40 weight part.The Cu powder additives of adding also can be used to the rate of combustion of thermite reaction, temperature of combustion and product purity.
Described Cu
2the granularity of O powder is preferably 200 ~ 300 orders.The granularity of described MgO powder is preferably 200 ~ 300 orders.Described CaF
2the granularity of powder is preferably 200 ~ 300 orders.The granularity of described Cu powder is preferably 200 ~ 300 orders.
The reaction adiabatic temperature of aluminothermy system Al-CuO, up to 3000K, makes the gas of thermite inside sharply expand, and causes the splash of product even to produce blast.Contact area between Al and CuO affects rate of combustion and the temperature of combustion of thermite reaction, and the granularity of Al powder and CuO powder is less, then contact area larger reaction Shaoxing opera is strong.The Al powder of the CuO powder adopting granular gradient to distribute in the present invention and granular gradient distribution, can be good at control combustion speed and temperature of combustion, reduces the splash rate of thermite reaction.
First the self-propagating combustion of thermite reaction needs the external world to provide certain energy to bring out topochemical reaction, and this process is called " lighting ".Reduce ignition temperature, to the reliability improving thermite reaction, there is important practical application.Al and Cu
2the self-propagating combustion that the Exotherm of O reacts for aluminothermy system further provides a large amount of heat.Add granularity in the present invention and be preferably 200 ~ 300 orders, be preferably the Cu of 2 ~ 6 weight parts
2o powder, reduces the ignition temperature of thermite reaction.
The thermal discharge of thermite reaction directly affects the severe degree of reaction and the density of product, for realizing the Effective Regulation to thermite reaction thermal discharge, in the present invention while control Al powder and the heat production of CuO powder granularity profile adjustment, with the addition of the thinner Cu powder that product purity can be kept to absorb heat in a large number again.Being preferably 200 ~ 300 orders by adding granularity, being preferably the thinner Cu powder of 0 ~ 40 weight part, having enriched the regulation and control to thermite reaction thermal discharge.
In the actual procedure of thermite reaction, heat production and radiating control the heat distribution of whole system, and the heat distribution of maintenance system stable equilibrium is conducive to the preparation of Cu-base composites.When utilizing high temperature, MgO is generated Mg by Al reduction and absorbs heat, and during low temperature, Mg is oxidized again the feature generating MgO heat release, can the heat distribution of good balanced aluminothermy system; And MgO and thermite reaction product A l
2o
3reaction generates MgAl
2o
4, melt viscosity can be regulated to promote being separated of metal and ceramic phase, not affect again the purity of metallographic phase.Add granularity in the present invention and be preferably 200 ~ 300 orders, weight part is preferably the MgO powder of 5 ~ 10 parts, the balanced heat distribution of aluminothermy system.
Slag former affects the important component that metal is separated with ceramic phase in thermite.Molten product after thermite reaction is Cu and Al
2o
3, due to Al
2o
3fusing point (2050 DEG C) far above the fusing point (1083 DEG C) of Cu, Al
2o
3to solidify prior to Cu and stay and wherein cannot be separated.Slag former CaF in the present invention
2the interpolation of powder, generates low melting point 3CaOAl in reaction system
2o
3mesophase spherule, makes melt viscosity reduce, and further promotes being separated and densification of metal and ceramic phase under the effect of super gravity field.Add granularity and be preferably 200 ~ 300 orders, weight part is preferably the CaF of 1 ~ 6 part
2powder, facilitates being separated and densification of metal and ceramic phase.
Thermite for hypergravity aid burning synthesis Cu-base composites of the present invention, when for the preparation of Cu-base composites, operation steps is as follows:
(1) raw material prepares: take various raw material by the formula of selected thermite, adopts ball mill under the condition of 50 ~ 100 revs/min, mix various raw material 30 ~ 60 minutes, obtains thermite;
(2) forming ingredient: step (1) is mixed the thermite compression moulding under 5 ~ 15MPa obtained; The size of thermite base substrate divides size to determine by used mould, and the diameter of thermite base substrate is generally within the scope of 20 ~ 200 millimeters;
(3) feed in mould: the thermite base substrate that the wild phase of the Cu-base composites that will prepare obtains by difference and the step (2) of preparation method is placed in graphite jig, quartz molds or corundum mould, and tungsten helix (diameter is 0.5 millimeter) is close to the surface of thermite base substrate upper end, and not with described contacting dies conducting;
(4) conbustion synthesis in super gravity field: be fixed in the reaction chamber of hypergravity aid burning synthesizer by the charging mould that step (3) obtains, connects tungsten helix circuit, off-response chamber; Start vacuum pump, vacuum tightness in reaction chamber is evacuated to 10-10000 pascal, close vacuum pump; Start the drive unit of hypergravity aid burning synthesizer, make reaction chamber high speed rotating until arrive 1000-5000 rev/min (gravity coefficient is 280 ~ 6990g); Starting ignition device, utilizes tungsten helix heating to bring out the Self-propagating Sintering Synthetic reaction of thermite in super gravity field; The drive unit of hypergravity aid burning synthesizer is closed after 10 ~ 30 minutes; After reaction chamber stops the rotation, venting valve to the air pressure of opening unit recovers a normal atmosphere; Open reaction chamber and take out product, product divides two-layer, and upper strata is ceramic phase product, and lower floor is the Cu-base composites product of design of components.
Thermite for hypergravity aid burning synthesis Cu-base composites of the present invention, the Al powder of the CuO powder adopting granular gradient to distribute in formula and granular gradient distribution, by adding Cu
2o, Cu, MgO and CaF
2the rate of combustion of reaction when Cu-base composites is prepared in regulation and control and thermal discharge, achieve stablizing of thermite reaction in super gravity field controlled.Thermite of the present invention has low splash rate, high thermal discharge, stablizes controlled feature, is applicable to the multiple Cu-base composites of hypergravity aid burning synthesis preparation.
Accompanying drawing explanation
Fig. 1. hypergravity aid burning synthesis schematic diagram.
Fig. 2. the photo of the hypergravity aid burning synthetic product of the embodiment of the present invention 1.
Fig. 3. the XRD figure spectrum of the hypergravity aid burning synthetic product of the embodiment of the present invention 1.
Embodiment
Embodiment 1
Thermite for hypergravity aid burning synthesis Cu-base composites is the Al powder of CuO powder and the granular gradient distribution distributed by granular gradient, and the Cu added
2o powder, MgO powder and CaF
2obtain after powder mixing; Composition and the proportioning of described thermite are as shown in table 1.
Table 1
The above-mentioned thermite for hypergravity aid burning synthesis Cu-base composites is utilized to prepare Cu-base composites:
(1) raw material prepares: take various raw material 200g altogether by the formula of the thermite in selected table 1, adopt ball mill under the condition of 50 revs/min, mix various raw material 60 minutes, obtain thermite;
(2) forming ingredient: step (1) is mixed the thermite obtained and be pressed into the thermite base substrate that diameter is 40 millimeters under 10MPa;
(3) feed in mould: prepare the graphite jig that diameter is 40 millimeters, be that the tungsten powder compacting of 2.5 microns is in the bottom of graphite jig by 100g granularity, the thermite base substrate that step (2) obtains is placed on tungsten powder, and tungsten helix (diameter is 0.5 millimeter) is close to the surface of thermite base substrate upper end, and do not contact conducting with graphite jig;
(4) conbustion synthesis in super gravity field: be fixed in the reaction chamber of hypergravity aid burning synthesizer by the charging mould that step (3) obtains, connects tungsten helix circuit, off-response chamber; Start vacuum pump, vacuum tightness in reaction chamber is evacuated to 200 pascals, close vacuum pump; Start the drive unit of hypergravity aid burning synthesizer, make reaction chamber high speed rotating until arrive 1890 revs/min (gravity coefficient is 1000g), hypergravity aid burning synthesis schematic diagram as shown in Figure 1; Starting ignition device, passes to the Self-propagating Sintering Synthetic reaction that thermite in super gravity field is brought out in 10 ampere electric current heatings to tungsten helix; The drive unit of hypergravity aid burning synthesizer is closed after 15 minutes; After reaction chamber stops the rotation, venting valve to the air pressure of opening unit recovers a normal atmosphere; Open reaction chamber and take out product, product divides two-layer, and as shown in Figure 2, upper strata product is MgAl
2o
4pottery (as shown in the A in Fig. 2), lower floor's product is tungsten-copper alloy (as shown in the B in Fig. 2); The MgAl that hypergravity aid burning synthesizes
2o
4the XRD figure spectrum of pottery and tungsten-copper alloy product as shown in Figure 3; Tungsten-copper alloy is after Linear cut and polishing, and adopting drainage to record density is 13.22g/cm
3, adopting three-point bending resistance method of testing (GB/T6569-86) to record bending strength is 1290MPa.
Embodiment 2
Thermite for hypergravity aid burning synthesis Cu-base composites is the Al powder of CuO powder and the granular gradient distribution distributed by granular gradient, and the Cu added
2o powder, Cu powder, MgO powder and CaF
2obtain after powder mixing; Composition and the proportioning of described thermite are as shown in table 2.
Table 2
The above-mentioned thermite for hypergravity aid burning synthesis Cu-base composites is utilized to prepare Cu-base composites:
(1) raw material prepares: take various raw material 200g altogether by the formula of the thermite in selected table 2, adopt ball mill under the condition of 50 revs/min, mix various raw material 60 minutes, obtain thermite;
(2) forming ingredient: step (1) is mixed the thermite obtained and be pressed into the thermite base substrate that diameter is 40 millimeters under 10MPa;
(3) feed in mould: prepare the graphite jig that diameter is 40 millimeters, be that the tungsten powder compacting of 2.5 microns is in the bottom of graphite jig by 50g granularity, the thermite base substrate that step (2) obtains is placed on tungsten powder, and tungsten helix (diameter is 0.5 millimeter) is close to the surface of thermite base substrate upper end, and do not contact conducting with graphite jig;
(4) conbustion synthesis in super gravity field: be fixed in the reaction chamber of hypergravity aid burning synthesizer by the charging mould that step (3) obtains, connects tungsten helix circuit, off-response chamber; Start vacuum pump, vacuum tightness in reaction chamber is evacuated to 200 pascals, close vacuum pump; Start the drive unit of hypergravity aid burning synthesizer, make reaction chamber high speed rotating until arrive 1680 revs/min (gravity coefficient is 800g); Starting ignition device, passes to the Self-propagating Sintering Synthetic reaction that thermite in super gravity field is brought out in 10 ampere electric current heatings to tungsten helix; The drive unit of hypergravity aid burning synthesizer is closed after 15 minutes; After reaction chamber stops the rotation, opening unit venting valve to air pressure recovers a normal atmosphere; Open reaction chamber and take out product, product divides two-layer, and upper strata product is MgAl
2o
4pottery, lower floor's product is tungsten-copper alloy; Tungsten-copper alloy is after Linear cut and polishing, and adopting drainage to record density is 12.86g/cm
3, adopting three-point bending resistance method of testing (GB/T6569-86) to record bending strength is 960MPa.
Embodiment 3
Thermite for hypergravity aid burning synthesis Cu-base composites is the Al powder of CuO powder and the granular gradient distribution distributed by granular gradient, and the Cu added
2o powder, Cu powder, MgO powder and CaF
2obtain after powder mixing; Composition and the proportioning of described thermite are as shown in table 3.
Table 3
The above-mentioned thermite for hypergravity aid burning synthesis Cu-base composites is utilized to prepare Cu-base composites:
(1) raw material prepares: take various raw material 200g altogether by the formula of the thermite in selected table 3, adopt ball mill under the condition of 100 revs/min, mix various raw material 30 minutes, obtain thermite;
(2) forming ingredient: step (1) is mixed the thermite obtained and be pressed into the thermite base substrate that diameter is 40 millimeters under 15MPa;
(3) feed in mould: prepare the graphite jig that diameter is 40 millimeters, be that the SiC powder-compacting of 75 microns is in the bottom of graphite jig by 30g granularity, the thermite base substrate that step (2) obtains is placed on SiC powder, and tungsten helix (diameter is 0.5 millimeter) is close to the surface of thermite base substrate upper end, and do not contact conducting with graphite jig;
(4) conbustion synthesis in super gravity field: be fixed in the reaction chamber of hypergravity aid burning synthesizer by the charging mould that step (3) obtains, connects tungsten helix circuit, off-response chamber; Start vacuum pump, vacuum tightness in reaction chamber is evacuated to 200 pascals, close vacuum pump; Start the drive unit of hypergravity aid burning synthesizer, make reaction chamber high speed rotating until arrive 1680 revs/min (gravity coefficient is 800g); Starting ignition device, passes to the Self-propagating Sintering Synthetic reaction that thermite in super gravity field is brought out in 10 ampere electric current heatings to tungsten helix; The drive unit of hypergravity aid burning synthesizer is closed after 20 minutes; After reaction chamber stops the rotation, opening unit venting valve to air pressure recovers a normal atmosphere; Open reaction chamber and take out product, product divides two-layer, and upper strata product is MgAl
2o
4and SiC ceramic, lower floor's product is SiC/Cu matrix material; SiC/Cu matrix material is after Linear cut and polishing, and adopting drainage to record density is 6.90g/cm
3, recording Rockwell hardness according to GB/T230.2 standard is 75HRB.
Embodiment 4
The present embodiment has investigated some important parameters under thermite static state (gravity coefficient is 1g): splash rate, namely the product reduction caused because of splash in thermite reaction process accounts for the percentage ratio of total mass, has the Mass lost of the thermite static reaction device of thermite to measure by thermite consumption and reaction fore and aft stowage; Rate of combustion, i.e. the distance of unit time combustion wavefront movement, the thermite reaction process being analyzed high-speed camera shooting by video software is recorded; Metal and ceramic separation case are learnt by the layering of observing response product and peel results.The weight part of each composition of the thermite for static thermite reaction is identical respectively with above-described embodiment 1,2,3, and gross weight is respectively 50g; The thermite base substrate that diameter is 40 millimeters is pressed into respectively under 10MPa, respectively thermite base substrate is loaded in thermite static reaction device, and tungsten helix (diameter is 0.5 millimeter) is close to the surface of thermite base substrate upper end, and do not contact conducting with thermite static reaction device, bring out thermite reaction to logical 10 ampere electric currents of tungsten helix.The result of thermite static reaction is as shown in table 4.
Table 4
Claims (6)
1. for a thermite for hypergravity aid burning synthesis Cu-base composites, it is characterized in that: Al powder, the Cu of the distribution of the CuO powder that described thermite is mainly distributed by granular gradient, granular gradient
2o powder, MgO powder and CaF
2obtain after powder mixing; Wherein: the granular gradient of the CuO powder of granular gradient distribution is distributed as 24 order > granularity>=100 orders, 100 order > granularity>=200 orders, 200 order > granularity>=300 orders; The granular gradient of the Al powder of granular gradient distribution is distributed as 30 order > granularity>=60 orders, 60 order > granularity>=100 orders, 100 order > granularity>=200 orders;
With the weight part of the CuO powder of the granular gradient distribution described in described thermite for benchmark, the CuO powder of the granular gradient distribution in described thermite is 35 ~ 75 weight parts, and the Al powder of granular gradient distribution is 8 ~ 12 weight parts, Cu
2o powder is 2 ~ 6 weight parts, and MgO powder is 5 ~ 10 weight parts, CaF
2powder is 1 ~ 6 weight part;
It is 2 ~ 40 weight parts that granular gradient in the CuO powder of described granular gradient distribution is distributed as 24 order > granularity >=100 object CuO powders, 100 order > granularity >=200 object CuO powders are 3 ~ 30 weight parts, and 200 order > granularity >=300 object CuO powders are 5 ~ 30 weight parts;
It is 2 ~ 8 weight parts that granular gradient in the Al powder of described granular gradient distribution is distributed as 30 order > granularity >=60 object Al powders, 60 order > granularity >=100 object Al powders are 2 ~ 4 weight parts, and 100 order > granularity >=200 object Al powders are 2 ~ 4 weight parts.
2. thermite according to claim 1, is characterized in that: described Cu
2the granularity of O powder is 200 ~ 300 orders; The granularity of described MgO powder is 200 ~ 300 orders; Described CaF
2the granularity of powder is 200 ~ 300 orders.
3. thermite according to claim 1, is characterized in that: containing Cu powder in described thermite.
4. thermite according to claim 3, it is characterized in that: containing Cu powder in described thermite, with the weight part of the CuO powder of the granular gradient distribution described in described thermite for benchmark, the content of described Cu powder in described thermite is 0 ~ 40 weight part.
5. thermite according to claim 3, is characterized in that: the granularity of described Cu powder is 200 ~ 300 orders.
6. thermite according to claim 4, is characterized in that: the granularity of described Cu powder is 200 ~ 300 orders.
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| CN105132724B (en) * | 2015-10-23 | 2018-01-26 | 攀枝花学院 | A kind of method that hypergravity auxiliary thermit reduction self- propagating prepares titanium-aluminium alloy |
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