CN103898345B - A kind of preparation method of molybdenum sodium alloy material - Google Patents
A kind of preparation method of molybdenum sodium alloy material Download PDFInfo
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- CN103898345B CN103898345B CN201410178165.8A CN201410178165A CN103898345B CN 103898345 B CN103898345 B CN 103898345B CN 201410178165 A CN201410178165 A CN 201410178165A CN 103898345 B CN103898345 B CN 103898345B
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Abstract
The invention provides a kind of preparation method of molybdenum sodium alloy material, comprise the following steps: one, prepare granulation molybdenum powder; Two, granulation molybdenum powder is carried out being pressed into base, then carry out sintering processes, obtain molybdenum skeleton; Three, Sodium orthomolybdate base is layed in molybdenum skeleton top, then carries out infiltration process, obtain semifinished material; Four, carry out Homogenization Treatments, obtain molybdenum sodium alloy material.Compared with preparing technique with traditional hot isostatic pressing, preparation technology of the present invention is easy to control more, low for equipment requirements, preparation cycle is short, prepared molybdenum sodium alloy materials microstructure and stable performance, and compactness is good, mass stably manufactured can be realized, be with a wide range of applications.
Description
Technical field
The invention belongs to molybdenum sodium alloy field of material technology, be specifically related to a kind of preparation method of molybdenum sodium alloy material.
Background technology
Along with the continuous exhaustion of the Nonrenewable energy resources such as oil, Sweet natural gas, various countries' researcher is devoted to the exploitation of renewable energy source.Sun power receives the concern of various countries as a kind of efficient, free of contamination renewable energy source.At present, the principal element that restriction solar film battery is significantly applied is exactly Cost Problems, reduces costs and just must improve photovoltaic effect, be i.e. electricity conversion.Molybdenum coating is applied to produce a kind of high-efficiency polycrystalline film photovoltaic cell, and this battery contains by CuInGaSe
2the absorption layer of composition, is therefore called CIGS photovoltaic cell.The structure of this battery is soda-lime glass deposited on substrates one deck molybdenum film, and then by CuInGaSe
2absorption layer attachment or growth are on molybdenum film.In early stage research discovery soda-lime glass substrate, a small amount of sodium ion penetrates molybdenum film and is diffused into CuInGaSe
2absorption layer, can improve the current carrying density of absorption layer, and then improve the energy conversion efficiency of this battery.In practical application, because molybdenum layer hinders the diffusion of Na, in film, Na component content is uncontrollable.Therefore, in order to effective control Na content, domestic and international researcher proposes pre-deposition one deck precursor NaF layer on Mo layer, such Na content just can be effectively controlled, but bringing a drawback is exactly current carrying density and adhesive equilibrium relationship, they are shifting relations, and NaF layer is once can not utilize completely, are easy to cause coming off of Mo layer and CIGS thin film layer.
Start emphatically research MoNa alloy target material in the recent period, this alloy target material deposits one deck MoNa alloy firm on the glass substrate, not only can effective control Na content, and avoids the danger using NaF layer to cause Mo layer and CIGS thin film pull-up to fall; And the result of study of reality also shows: MoNa alloy is as the Na source of CIGS solar film battery, and have the ability of the absorption Na higher than NaF layer, electricity conversion is higher.And substrate is unrestricted, adopts flexible substrate that battery can be made lighter, also more easily make different shape.
As can be seen here, in photovoltaic application, the possibility that molybdenum sodium material replaces pure molybdenum is very large, but its to prepare difficulty also very large.Analyze theoretically, the fusing point difference of molybdenum and sodium is comparatively large, and the fusing point of molybdenum is 2620 ± 10 DEG C, and the fusing point of sodium is 98 DEG C; Boiling point differs more, and the boiling point of molybdenum is 4639 DEG C; The boiling point of sodium is 883 DEG C.At present, have the method for report to be first adopt the method for mist projection granulating to prepare molybdenum sodium alloy powder, then hot isostatic pressing becomes molybdenum sodium alloy goods, then prepares by the method for sintering the molybdenum sodium alloy target having certain density He meet performance requriements.The shortcoming of the method is that equipment cost is high, operation is numerous and diverse, energy consumption is large and production efficiency is low, is difficult to realize batch production.
Therefore, need a kind of can low cost, less energy-consumption the novel process of molybdenum sodium alloy material can be prepared efficiently.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of preparation method of molybdenum sodium alloy material.After the method is different from mist projection granulating hot isostatic pressing reburn knot traditional processing mode, belong to a kind of new technology route preparing molybdenum sodium alloy material.The method adopts the method for infiltration, with low cost, less energy-consumption, prepares superior in quality molybdenum sodium alloy material efficiently, can realize the mass production of molybdenum sodium alloy material.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of molybdenum sodium alloy material, and it is characterized in that, the method comprises the following steps:
Step one, granulation is carried out to molybdenum powder, obtain granulation molybdenum powder;
Step 2, the molybdenum powder of granulation described in step one is pressed into molybdenum base, then protected at hydrogen atmosphere by molybdenum base, temperature is be incubated 60min ~ 120min under the condition of 1100 DEG C ~ 1300 DEG C to carry out sintering processes, obtains the molybdenum skeleton that porosity is 25% ~ 40%;
Step 3, Sodium orthomolybdate powder is pressed into Sodium orthomolybdate base, again Sodium orthomolybdate base is layed in the skeleton of molybdenum described in step 2 top, then molybdenum skeleton top being equipped with Sodium orthomolybdate base is protected at hydrogen atmosphere, temperature is be incubated 60min ~ 90min under the condition of 800 DEG C ~ 1000 DEG C to carry out infiltration process, obtains semifinished material; The actual weight n of described Sodium orthomolybdate base is theoretical weight n
01.05 ~ 1.2 times, the theoretical weight n of described Sodium orthomolybdate base
0pass through formula
calculate, wherein m is the weight of molybdenum skeleton, and the weight percentage of the unit of m to be g, x be sodium in molybdenum sodium alloy material to be prepared, the unit of x is %, n and n
0unit be g;
Step 4, protected at hydrogen atmosphere by semifinished material described in step 3, temperature is be incubated 60min ~ 120min under the condition of 700 DEG C ~ 900 DEG C to carry out Homogenization Treatments, obtains molybdenum sodium alloy material after naturally cooling; In described molybdenum sodium alloy material, the weight percentage of sodium is 2.5% ~ 4.5%.
The preparation method of above-mentioned a kind of molybdenum sodium alloy material, is characterized in that, the Fisher particle size of molybdenum powder described in step one is 4.5 μm ~ 6 μm, and loose density is 1.5g/cm
3~ 3.0g/cm
3.
The preparation method of above-mentioned a kind of molybdenum sodium alloy material, it is characterized in that, the detailed process of granulation described in step one is: by molybdenum powder, paraffin and aviation spirit solution in mass ratio 100: (0.3 ~ 0.5): (0.5 ~ 1.0) adds ball milling granulation 6h ~ 8h in ball grinder, obtains granulation molybdenum powder.
The preparation method of above-mentioned a kind of molybdenum sodium alloy material, is characterized in that, the solution of aviation spirit described in step one by aviation spirit and deionized water in mass ratio (5 ~ 6): (94 ~ 95) mix and form.
The preparation method of above-mentioned a kind of molybdenum sodium alloy material, is characterized in that, the thickness of the skeleton of molybdenum described in step 2 is 60mm ~ 70mm.
The present invention compared with prior art has the following advantages:
1, first the present invention carries out the process of molybdenum powder granulation.The granularity of molybdenum powder should be comparatively even, and granularity is crossed conference and caused pressed compact hole uneven, causes the enrichment of Sodium orthomolybdate; Too small, easily there is particle agglomeration, cause skeleton passage to close or blocking, cause Sodium orthomolybdate skewness; Priority limit of the present invention fixes within the scope of 4.5 ~ 6 μm.In addition, the loose density of molybdenum powder should be relatively larger, is because coarse grained macrovoid can be filled by a part of fine particle, makes the even pore distribution of pressed compact, reduce the defects such as the zone of enrichment that forms Sodium orthomolybdate in follow-up infiltration and shrinkage cavity; The present invention is preferably limited to 1.5g/cm
3~ 3.0g/cm
3in scope.
2, in order to improve the compactibility of molybdenum base, make the density distribution of porous molybdenum skeleton as far as possible evenly and form certain space, it is lubricant that the present invention adds volatile paraffin in ball milling mixing process, and add aviation spirit solution, be conducive to the intensity improving porous pressed compact, reduce the compacting such as layering and cracking waste product.Because paraffin and aviation spirit can not react with molybdenum or dissolve, paraffin and aviation spirit are evenly distributed between molybdenum powder particle, sinter in the process of molybdenum skeleton for a long time at high temperature, along with constantly volatilizing or resolving into gas effusion, effectively can prevent the agglomeration between molybdenum particle, molybdenum skeleton has and is evenly distributed and mutually through communicating passage.The interpolation of aviation spirit, not only makes molybdenum matrix porosity mutually through, and pore texture more rationally evenly, and can strengthen the intensity of pressed compact, avoids in follow-up infiltration process and occurs structure collapse phenomenon.
3, the present invention sinters after being pressed into base to granulation molybdenum powder, by controlling sintering process, the additive in granulation molybdenum powder can be removed on the one hand, increasing the intensity of molybdenum skeleton on the other hand, be beneficial to the carrying out of follow-up infiltration, finally obtain the molybdenum skeleton with certain porosity.
4, infiltration is one critical process that the present invention prepares molybdenum sodium alloy material, and the quality of infiltration process is directly connected to the height of quality product, and affects processing and the use of subsequent product.In infiltration method sintering process, the densification of molybdenum sodium alloy is mainly by the intraskeletal capillary force of molybdenum, when temperature reaches more than Sodium orthomolybdate fusing point, the pressure ratio external world in kapillary is little, and under capillary force action, the Sodium orthomolybdate of liquid phase is pressed in the intraskeletal perforate of molybdenum.The present invention fully takes into account the vaporization at high temperature of Sodium orthomolybdate, after a large amount of creative research, by more than theoretical amount for the actual add-on of Sodium orthomolybdate 5 ~ 20%.And according to the fusing point of Sodium orthomolybdate at about 650 DEG C, therefore, formulating infiltration process is: be heated to 800 DEG C ~ 1000 DEG C under hydrogen shield, soaking time 60min ~ 90min, finally realize excellent infiltration effect.
5, the present invention carries out Homogenization Treatments after infiltration, can make the distribution uniformity more of the Sodium orthomolybdate of infiltration sample inside.
6, the preparation method of molybdenum sodium alloy material of the present invention, technical process is short, and technique is easy to control, and material structure and stable performance, have obvious cost advantage.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the metallographic structure photo of molybdenum sodium alloy material prepared by the embodiment of the present invention 1.
Fig. 2 is the metallographic structure photo of molybdenum sodium alloy material prepared by the embodiment of the present invention 2.
Fig. 3 is the metallographic structure photo of molybdenum sodium alloy material prepared by the embodiment of the present invention 3.
Fig. 4 is the metallographic structure photo of molybdenum sodium alloy material prepared by the embodiment of the present invention 4.
Fig. 5 is the metallographic structure photo of molybdenum sodium alloy material prepared by the embodiment of the present invention 5.
Embodiment
Embodiment 1
The preparation of molybdenum sodium alloy material:
Step one, molybdenum powder, paraffin and aviation spirit solution are added in ball grinder ball milling granulation 8h in mass ratio at 100: 0.5: 1, obtain granulation molybdenum powder, the Fisher particle size of described molybdenum powder is 5.6 μm, and loose density is 1.8g/cm
3; Described aviation spirit solution in mass ratio by aviation spirit and deionized water is mixed forms at 6: 94;
Step 2, the molybdenum powder of granulation described in step one is pressed into molybdenum base, then molybdenum base is placed in hydrogen furnace, in hydrogen atmosphere protection, temperature is be incubated 120min under the condition of 1200 DEG C to carry out sintering processes, and obtaining porosity is 30%, and thickness is the molybdenum skeleton of 65mm; In specific implementation process, can granulation molybdenum powder be loaded in punching block, adopt the method for limit for height compacting to make the relative density of molybdenum base control about 67%, realize shrinking on a small quantity through sintering process thus reach the porosity of 30%;
Step 3, Sodium orthomolybdate powder is pressed into Sodium orthomolybdate base, again Sodium orthomolybdate base is layed in the skeleton of molybdenum described in step 2 top, then molybdenum skeleton top being equipped with Sodium orthomolybdate base is put into graphite jig and is placed on hydrogen furnace, protect at hydrogen atmosphere, temperature is be incubated 60min under the condition of 950 DEG C to carry out infiltration process, obtains semifinished material; The actual weight n of described Sodium orthomolybdate base is theoretical weight n
01.1 times, the theoretical weight n of described Sodium orthomolybdate base
0pass through formula
calculate, wherein m is the weight of molybdenum skeleton, the weight percentage of the unit of m to be g, x be sodium in molybdenum sodium alloy material to be prepared, x=3.0%, m=3000g in the present embodiment, the actual weight n=512g of Sodium orthomolybdate base;
Step 4, semifinished material described in step 3 is placed in hydrogen furnace, in hydrogen atmosphere protection, temperature is be incubated 90min under the condition of 800 DEG C to carry out Homogenization Treatments, obtains molybdenum sodium alloy material after naturally cooling.
As shown in Figure 1, in figure, white portion is Sodium orthomolybdate to the metallographic structure photo of molybdenum sodium alloy material prepared by the present embodiment, and black region is molybdenum.As shown in Figure 1, in the molybdenum sodium alloy material prepared of the present embodiment, molybdenum and Sodium orthomolybdate realize homogenizing and distribute.After testing, in molybdenum sodium alloy material prepared by the present embodiment, the actual weight percentage composition of sodium is 3%, and compactness is good, and match with design requirements, material structure and stable performance, can realize mass stably manufactured, be with a wide range of applications.
Embodiment 2
The preparation of molybdenum sodium alloy material:
Step one, molybdenum powder, paraffin and aviation spirit solution are added in ball grinder ball milling granulation 6h in mass ratio at 100: 0.5: 0.5, obtain granulation molybdenum powder, the Fisher particle size of described molybdenum powder is 4.5 μm, and loose density is 1.5g/cm
3; Described aviation spirit solution in mass ratio by aviation spirit and deionized water is mixed forms at 5: 95;
Step 2, the molybdenum powder of granulation described in step one is pressed into molybdenum base, then molybdenum base is placed in hydrogen furnace, in hydrogen atmosphere protection, temperature is be incubated 120min under the condition of 1100 DEG C to carry out sintering processes, and obtaining porosity is 25%, and thickness is the molybdenum skeleton of 60mm; In specific implementation process, granulation molybdenum powder is loaded in punching block, adopt the method for limit for height compacting to make the relative density of molybdenum base control about 72%, realize shrinking on a small quantity through sintering process thus reach the porosity of 25%;
Step 3, Sodium orthomolybdate powder is pressed into Sodium orthomolybdate base, again Sodium orthomolybdate base is layed in the skeleton of molybdenum described in step 2 top, then molybdenum skeleton top being equipped with Sodium orthomolybdate base is put into graphite jig and is placed on hydrogen furnace, protect at hydrogen atmosphere, temperature is be incubated 80min under the condition of 900 DEG C to carry out infiltration process, obtains semifinished material; The actual weight n of described Sodium orthomolybdate base is theoretical weight n
01.05 times, the theoretical weight n of described Sodium orthomolybdate base
0pass through formula
calculate, wherein m is the weight of molybdenum skeleton, the weight percentage of the unit of m to be g, x be sodium in molybdenum sodium alloy material to be prepared, x=2.5%, m=3000g in the present embodiment, the actual weight n=397g of Sodium orthomolybdate base;
Step 4, semifinished material described in step 3 is placed in hydrogen furnace, in hydrogen atmosphere protection, temperature is be incubated 80min under the condition of 700 DEG C to carry out Homogenization Treatments, obtains molybdenum sodium alloy material after naturally cooling.
As shown in Figure 2, in figure, white portion is Sodium orthomolybdate to the metallographic structure photo of molybdenum sodium alloy material prepared by the present embodiment, and black region is molybdenum.As shown in Figure 2, in the molybdenum sodium alloy material prepared of the present embodiment, molybdenum and Sodium orthomolybdate realize homogenizing and distribute.After testing, in molybdenum sodium alloy material prepared by the present embodiment, the actual weight percentage composition of sodium is 2.5%, and compactness is good, and match with design requirements, material structure and stable performance, can realize mass stably manufactured, be with a wide range of applications.
Embodiment 3
The preparation of molybdenum sodium alloy material:
Step one, molybdenum powder, paraffin and aviation spirit solution are added in ball grinder ball milling granulation 7h in mass ratio at 100: 0.3: 0.5, obtain granulation molybdenum powder, the Fisher particle size of described molybdenum powder is 5.2 μm, and loose density is 2.1g/cm
3; Described aviation spirit solution in mass ratio by aviation spirit and deionized water is mixed forms at 5: 94;
Step 2, the molybdenum powder of granulation described in step one is pressed into molybdenum base, then molybdenum base is placed in hydrogen furnace, in hydrogen atmosphere protection, temperature is be incubated 90min under the condition of 1200 DEG C to carry out sintering processes, and obtaining porosity is 28%, and thickness is the molybdenum skeleton of 70mm; In specific implementation process, granulation molybdenum powder is loaded in punching block, after adopting the method for limit for height compacting to make compacting, the relative density of molybdenum base controls about 70%, realizes shrinking on a small quantity thus reach the porosity of 28% through sintering process;
Step 3, Sodium orthomolybdate powder is pressed into Sodium orthomolybdate base, again Sodium orthomolybdate base is layed in the skeleton of molybdenum described in step 2 top, then molybdenum skeleton top being equipped with Sodium orthomolybdate base is put into graphite jig and is placed on hydrogen furnace, protect at hydrogen atmosphere, temperature is be incubated 80min under the condition of 1000 DEG C to carry out infiltration process, obtains semifinished material; The actual weight n of described Sodium orthomolybdate base is theoretical weight n
01.2 times, the theoretical weight n of described Sodium orthomolybdate base
0pass through formula
calculate, wherein m is the weight of molybdenum skeleton, the weight percentage of the unit of m to be g, x be sodium in molybdenum sodium alloy material to be prepared, x=2.8%, m=3000g in the present embodiment, the actual weight n=516g of Sodium orthomolybdate base;
Step 4, semifinished material described in step 3 is placed in hydrogen furnace, in hydrogen atmosphere protection, temperature is be incubated 60min ~ 120min under the condition of 700 DEG C ~ 900 DEG C to carry out Homogenization Treatments, obtains molybdenum sodium alloy material after naturally cooling.
As shown in Figure 3, in figure, white portion is Sodium orthomolybdate to the metallographic structure photo of molybdenum sodium alloy material prepared by the present embodiment, and black region is molybdenum.As shown in Figure 3, in the molybdenum sodium alloy material prepared of the present embodiment, molybdenum and Sodium orthomolybdate realize homogenizing and distribute.After testing, in molybdenum sodium alloy material prepared by the present embodiment, the actual weight percentage composition of sodium is 2.7%, and compactness is good, and match with design requirements, material structure and stable performance, can realize mass stably manufactured, be with a wide range of applications.
Embodiment 4
The preparation of molybdenum sodium alloy material:
Step one, molybdenum powder, paraffin and aviation spirit solution are added in ball grinder ball milling granulation 8h in mass ratio at 100: 0.3: 1.0, obtain granulation molybdenum powder, the Fisher particle size of described molybdenum powder is 6 μm, and loose density is 3.0g/cm
3; Described aviation spirit solution in mass ratio by aviation spirit and deionized water is mixed forms at 6: 95;
Step 2, the molybdenum powder of granulation described in step one is pressed into molybdenum base, then molybdenum base is placed in hydrogen furnace, in hydrogen atmosphere protection, temperature is be incubated 60min under the condition of 1300 DEG C to carry out sintering processes, and obtaining porosity is 26%, and thickness is the molybdenum skeleton of 64mm; In specific implementation process, granulation molybdenum powder is loaded in punching block, after adopting the method for limit for height compacting to make compacting, the relative density of molybdenum base controls about 72%, realizes shrinking on a small quantity thus reach the porosity of 26% through sintering process;
Step 3, Sodium orthomolybdate powder is pressed into Sodium orthomolybdate base, again Sodium orthomolybdate base is layed in the skeleton of molybdenum described in step 2 top, then molybdenum skeleton top being equipped with Sodium orthomolybdate base is put into graphite jig and is placed on hydrogen furnace, protect at hydrogen atmosphere, temperature is be incubated 60min under the condition of 1000 DEG C to carry out infiltration process, obtains semifinished material; The actual weight n of described Sodium orthomolybdate base is theoretical weight n
01.15 times, the theoretical weight n of described Sodium orthomolybdate base
0pass through formula
calculate, wherein m is the weight of molybdenum skeleton, the weight percentage of the unit of m to be g, x be sodium in molybdenum sodium alloy material to be prepared, in the present embodiment, and x=2.6%, m=3000g, the actual weight n=455g of Sodium orthomolybdate base;
Step 4, semifinished material described in step 3 is placed in hydrogen furnace, in hydrogen atmosphere protection, temperature is be incubated 60min ~ 120min under the condition of 700 DEG C ~ 900 DEG C to carry out Homogenization Treatments, obtains molybdenum sodium alloy material after naturally cooling.
As shown in Figure 4, Sodium orthomolybdate and molybdenum good knitting in figure, without obviously demarcating for the metallographic structure photo of molybdenum sodium alloy material prepared by the present embodiment.As shown in Figure 4, in the molybdenum sodium alloy material prepared of the present embodiment, molybdenum and Sodium orthomolybdate realize homogenizing and distribute.After testing, in molybdenum sodium alloy material prepared by the present embodiment, the actual weight percentage composition of sodium is 2.6%, and compactness is good, and match with design requirements, material structure and stable performance, can realize mass stably manufactured, be with a wide range of applications.
Embodiment 5
The preparation of molybdenum sodium alloy material:
Step one, molybdenum powder, paraffin and aviation spirit solution are added in ball grinder ball milling granulation 7h in mass ratio at 100: 0.4: 0.8, obtain granulation molybdenum powder, the Fisher particle size of described molybdenum powder is 5.5 μm, and loose density is 2.4g/cm
3; Described aviation spirit solution in mass ratio by aviation spirit and deionized water is mixed forms at 5.5: 94.5;
Step 2, the molybdenum powder of granulation described in step one is pressed into molybdenum base, then molybdenum base is placed in hydrogen furnace, in hydrogen atmosphere protection, temperature is be incubated 100min under the condition of 1150 DEG C to carry out sintering processes, and obtaining porosity is 40%, and thickness is the molybdenum skeleton of 68mm; In specific implementation process, granulation molybdenum powder is loaded in punching block, after adopting the method for limit for height compacting to make compacting, the relative density of molybdenum base controls about 58%, realizes shrinking on a small quantity thus reach the porosity of 40% through sintering process;
Step 3, Sodium orthomolybdate powder is pressed into Sodium orthomolybdate base, again Sodium orthomolybdate base is layed in the skeleton of molybdenum described in step 2 top, then molybdenum skeleton top being equipped with Sodium orthomolybdate base is put into graphite jig and is placed on hydrogen furnace, protect at hydrogen atmosphere, temperature is be incubated 70min under the condition of 900 DEG C to carry out infiltration process, obtains semifinished material; The actual weight n of described Sodium orthomolybdate base is theoretical weight n
01.2 times, the theoretical weight n of described Sodium orthomolybdate base
0pass through formula
calculate, wherein m is the weight of molybdenum skeleton, the weight percentage of the unit of m to be g, x be sodium in molybdenum sodium alloy material to be prepared, in the present embodiment, and x=4.5%, m=3000g, the actual weight n=908g of Sodium orthomolybdate base;
Step 4, semifinished material described in step 3 is placed in hydrogen furnace, in hydrogen atmosphere protection, temperature is be incubated 100min under the condition of 700 DEG C to carry out Homogenization Treatments, obtains molybdenum sodium alloy material after naturally cooling.
As shown in Figure 5, Sodium orthomolybdate and molybdenum good knitting in figure, without obviously demarcating for the metallographic structure photo of molybdenum sodium alloy material prepared by the present embodiment.As shown in Figure 5, in the molybdenum sodium alloy material prepared of the present embodiment, molybdenum and Sodium orthomolybdate realize homogenizing and distribute.After testing, in molybdenum sodium alloy material prepared by the present embodiment, the actual weight percentage composition of sodium is 4.5%, and compactness is good, and match with design requirements, material structure and stable performance, can realize mass stably manufactured, be with a wide range of applications.
The above is only preferred embodiment of the present invention, not imposes any restrictions the present invention.Every above embodiment is done according to invention technical spirit any simple modification, change and equivalence change, all still belong in the protection domain of technical solution of the present invention.
Claims (4)
1. a preparation method for molybdenum sodium alloy material, is characterized in that, the method comprises the following steps:
Step one, granulation is carried out to molybdenum powder, obtain granulation molybdenum powder; The detailed process of described granulation is: by molybdenum powder, paraffin and aviation spirit solution in mass ratio 100: (0.3 ~ 0.5): (0.5 ~ 1.0) adds ball milling granulation 6h ~ 8h in ball grinder, obtains granulation molybdenum powder;
Step 2, the molybdenum powder of granulation described in step one is pressed into molybdenum base, then protected at hydrogen atmosphere by molybdenum base, temperature is be incubated 60min ~ 120min under the condition of 1100 DEG C ~ 1300 DEG C to carry out sintering processes, obtains the molybdenum skeleton that porosity is 25% ~ 40%;
Step 3, Sodium orthomolybdate powder is pressed into Sodium orthomolybdate base, again Sodium orthomolybdate base is layed in the skeleton of molybdenum described in step 2 top, then molybdenum skeleton top being equipped with Sodium orthomolybdate base is protected at hydrogen atmosphere, temperature is be incubated 60min ~ 90min under the condition of 800 DEG C ~ 1000 DEG C to carry out infiltration process, obtains semifinished material; The actual weight n of described Sodium orthomolybdate base is theoretical weight n
01.05 ~ 1.2 times, the theoretical weight n of described Sodium orthomolybdate base
0pass through formula
calculate, wherein m is the weight of molybdenum skeleton, and the weight percentage of the unit of m to be g, x be sodium in molybdenum sodium alloy material to be prepared, the unit of x is %, n and n
0unit be g;
Step 4, protected at hydrogen atmosphere by semifinished material described in step 3, temperature is be incubated 60min ~ 120min under the condition of 700 DEG C ~ 900 DEG C to carry out Homogenization Treatments, obtains molybdenum sodium alloy material after naturally cooling; In described molybdenum sodium alloy material, the weight percentage of sodium is 2.5% ~ 4.5%.
2. the preparation method of a kind of molybdenum sodium alloy material according to claim 1, is characterized in that, the Fisher particle size of molybdenum powder described in step one is 4.5 μm ~ 6 μm, and loose density is 1.5g/cm
3~ 3.0g/cm
3.
3. the preparation method of a kind of molybdenum sodium alloy material according to claim 1, is characterized in that, the solution of aviation spirit described in step one by aviation spirit and deionized water in mass ratio (5 ~ 6): (94 ~ 95) mix and form.
4. the preparation method of a kind of molybdenum sodium alloy material according to claim 1, is characterized in that, the thickness of the skeleton of molybdenum described in step 2 is 60mm ~ 70mm.
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| CN107794399B (en) * | 2017-10-13 | 2022-03-15 | 浙江福达合金材料科技有限公司 | Preparation method of superfine high-dispersion silver-tungsten electrical contact material |
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