CN104117685B - A kind of preparation method of sodium molybdate doped molybdenum - Google Patents
A kind of preparation method of sodium molybdate doped molybdenum Download PDFInfo
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- CN104117685B CN104117685B CN201410369881.4A CN201410369881A CN104117685B CN 104117685 B CN104117685 B CN 104117685B CN 201410369881 A CN201410369881 A CN 201410369881A CN 104117685 B CN104117685 B CN 104117685B
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Abstract
The invention provides the preparation method of a kind of sodium molybdate doped molybdenum, comprise the following steps: one, polyacrylamide is added in deionized water and be sufficiently stirred for, until polyacrylamide is completely dissolved, obtain binding agent；Two, molybdenum powder and sodium molybdate powder are added mix homogeneously in binding agent, obtain slurry；Three, utilize spray drying tower that step slurry is carried out spray drying treatment, obtain pellet；Four, under the protection of hydrogen atmosphere, pellet is carried out carbonization treatment, after natural cooling, obtain sodium molybdate doped molybdenum.The present invention uses that addition is few, intermiscibility good, low temperature is easily got rid of and can meet the polyacrylamide of pelletize requirement and is configured to bonding agent, requires low to raw materials for production, and technique is easily controllable, easy and simple to handle, safety, is suitable to large-scale production.Using sodium molybdate doped molybdenum prepared by the present invention, product Oxygen potential is high, and Organic substance is readily removed, and carbon content is low, good product consistency, can meet the requirement to powder of the special forming mode completely.
Description
Technical field
The invention belongs to Mo processing technique field, be specifically related to the system of a kind of sodium molybdate doped molybdenum
Preparation Method.
Background technology
Energy crisis, environmental pollution are the significant challenge that the mankind are faced with greenhouse effect, develop new energy
Source and renewable and clean energy resource become one of 21 century technical field most determining impact.At present,
Apply the most universal fossil energy, its limited amount, and will be exhausted.The explored stone in the whole world
Oilreserves can only use the year two thousand twenty, and natural gas can only be used about the year two thousand forty, and coal also can only maintain
100 or two hundred years.Therefore, in order to maintain the survival and development of the mankind, Looking For Substitutions Of Oil is to solve future
Mankind's demand to the energy has become the matter of great urgency with the protection to environment.Solar energy be one take no
To the greatest extent, nexhaustible renewable and clean energy resource, as one of the important means of Solar use, to too
The research and development of sun energy battery also become to become more and more important.
At present, as thin-film solar cells most with prospects, CIGS (CIGS) thin film
Photovoltaic products is with the high absorption coefficient of light, high transformation efficiency, high stability, adjustable energy gap, relatively
The advantages such as strong capability of resistance to radiation constantly seize the market share, will become a new generation's high-efficiency solar electricity
The main product in pond.
Owing to Na is useful to photovoltaic property, electricity conversion can be improved, it is contemplated that in substrate
Na is diffused in CIGS thin film, and the general underlay substrate used is plating molybdenum alkali glass, and some producers are also
The another deposition compound containing Na is used to control the content of Na.But all these all there is operation
Various and technology controlling and process point increases the unfavorable drawback brought, and therefore, the most existing a lot of photovoltaic enterprises turn
For seeking the alloy material of a kind of molybdenum and sodium, in the way of more efficient and low cost, prepare high turning
Change the thin-film solar cells of efficiency.
Owing to molybdenum and the fusing point of sodium and density variation are relatively big, conventional preparation technology can not meet will
Ask, and some special forming mode such as hot spray process etc., need raw material is carried out pretreatment, its mesh
Be provided to reduce the densification energy barrier of this powder body so that it is have in forming process enough intensity and
Density.Special forming mode requires that raw material powder particle size is uniformly (about 10 μm), it is ensured that uniform
Dispersion, good mobility and bigger sintering rate, powder particle is subsphaeroidal, and specific surface is big.
Common molybdenum powder is irregular due to granule-morphology, poor fluidity, reunites serious, it is impossible to meet special one-tenth
The requirement to body of powder performance of the shape mode.Accordingly, it would be desirable to molybdenum powder is doped, and carry out spray dried
Dry pelletize processes.
General molybdenum powder pelletize binding agent be mass percent concentration be the vinyl alcohol of 10%～15%
(PVA) solution, the addition of PVA is big, therefore to the carbon that removing PVA brings into, need with
After carry out high temperature decarburization (general temperature is more than 900 DEG C).Owing to target is tight to the requirement of carbon content
Lattice (generally no greater than 50ppm), and after adding PVA, in order to reach this requirement, need relatively
The decarburization time of high decarburization temperature or longer, could lower carbon content, but the highest taking off
The drawback the most serious that carbon temperature is brought is exactly that the compound of sodium can volatilize in a large number, and can cause
The uneven distribution of Na in powder body.
Therefore, need research and development a kind of product Oxygen potential height badly, Organic substance is readily removed, carbon content is low, product
The preparation method of the sodium molybdate doped molybdenum that product concordance is good.
Summary of the invention
The technical problem to be solved is for above-mentioned the deficiencies in the prior art, it is provided that a kind of
The preparation method of sodium molybdate doped molybdenum.Addition is few, intermiscibility good, low temperature is easily arranged in the method employing
Except the polyacrylamide that can meet again pelletize requirement is configured to bonding agent, raw materials for production are required low, to behaviour
Making personnel's health not injure, technique is easily controllable, and easy and simple to handle, safety is suitable to large-scale production.
Using sodium molybdate doped molybdenum prepared by the method, product Oxygen potential is high, and Organic substance is readily removed, carbon
Content is low, good product consistency, can meet the requirement to powder of the special forming mode completely.
For solving above-mentioned technical problem, the technical solution used in the present invention is: a kind of sodium molybdate doping molybdenum
The preparation method of powder, it is characterised in that the method comprises the following steps:
Step one, polyacrylamide is added in deionized water it is sufficiently stirred for, until polyacrylamide is complete
CL, obtains binding agent；The addition of described polyacrylamide is to add in every liter of deionized water
3g～5g polyacrylamide；
Step 2, molybdenum powder and sodium molybdate powder are added described in step one mix homogeneously in binding agent,
To slurry；The addition of described molybdenum powder is addition 2kg～4kg molybdenum powder, described molybdic acid in every liter of binding agent
The addition of sodium powder is according to the weight/mass percentage composition conversion of sodium in sodium molybdate doped molybdenum to be prepared
Obtain；
Step 3, utilize spray drying tower that slurry described in step 2 is carried out spray drying treatment,
To pellet；
Step 4, under the protection of hydrogen atmosphere, by pellet described in step 3 in temperature be
It is incubated 1.5h～2.5h under conditions of 600 DEG C～700 DEG C and carries out carbonization treatment, after natural cooling, obtain molybdic acid
Natrium doping molybdenum powder；In described sodium molybdate doped molybdenum, the weight/mass percentage composition of sodium is 1%～5%, carbon
Mass content is not higher than 50ppm.
The preparation method of above-mentioned a kind of sodium molybdate doped molybdenum, it is characterised in that described in step 3
The concrete technology parameter of spray drying treatment is: the intake air temperature of spray drying tower is
200 DEG C～240 DEG C, air outlet temperature is 110 DEG C～150 DEG C, and in spray drying tower, the rotating speed of nebulizer is
1.0×104R/min～1.3 × 104r/min。
The preparation method of above-mentioned a kind of sodium molybdate doped molybdenum, it is characterised in that spray drying tower
Intake air temperature is 220 DEG C, and air outlet temperature is 130 DEG C, the rotating speed of nebulizer in spray drying tower
It is 1.1 × 104r/min。
The present invention compared with prior art has the advantage that
1, the present invention selects that addition is few, intermiscibility good, low temperature is easily got rid of and can meet the poly-of pelletize requirement
Acrylamide is configured to bonding agent, makes full use of its viscosity big, at a temperature of the decarburization of 600～700 DEG C i.e.
Can all get rid of, owing to its addition is few, after carbonization treatment, carbon content is not higher than 50ppm, complete
Entirely can meet the requirement to composition carbon content of the molybdenum sodium alloy target.
2, the low-temperature sintering process of pellet after carbonization treatment i.e. pelletize, adds in the mainly removing pelletize of its purpose
The caking property Organic substance entered, and eliminate the internal stress of powder, make the sodium molybdate distribution within powder more equal
Even unanimously.For using the binding agent of polyacrylamide preparation, decarburization temperature is low, it is possible to effectively keep away
Exempt from the existence of the reduction problem of the sodium content that traditional high temperature carbonization treatment causes.
3, the present invention is after a large amount of creative experiments and optimization, and final employing polyacrylamide is configured to glue
Knot agent, and it is configured to the slurry of suitable viscosity, then spray dried with molybdenum powder and sodium molybdate powder with certain proportion
Dry process, it is thus achieved that by the cluster of grains powder of many granule bondings, then these cluster of grains powder are taken off
Carbon processes, thus acquisition has certain size and the big granularity of irregular figure, the sodium molybdate of high fluidity are mixed
Miscellaneous molybdenum powder.
4, raw materials for production are required low by the present invention, the organic adhesive material-polyacrylamide amine value used
Lattice are cheap, not injure operator's health.Its technique is easily controllable, easy and simple to handle, safety,
Be suitable to large-scale production.Sodium molybdate doped molybdenum prepared by the present invention, product Oxygen potential is high, Organic substance
Readily removed, carbon content is low, good product consistency, can meet special forming mode completely to powder
Requirement.
With embodiment, the present invention is described in further detail below in conjunction with the accompanying drawings.
Accompanying drawing explanation
Fig. 1 is the metallographic structure figure of the sodium molybdate doped molybdenum of the embodiment of the present invention 1 preparation.
Fig. 2 is the metallographic structure figure of the sodium molybdate doped molybdenum of the embodiment of the present invention 2 preparation.
Fig. 3 is the metallographic structure figure of the sodium molybdate doped molybdenum of the embodiment of the present invention 3 preparation.
Detailed description of the invention
Embodiment 1
The preparation method of the present embodiment sodium molybdate doped molybdenum comprises the following steps:
Step one, polyacrylamide is added in deionized water it is sufficiently stirred for, until polyacrylamide is complete
CL, obtains binding agent；The addition of described polyacrylamide is addition 4g in every liter of deionized water
Polyacrylamide；
Step 2, molybdenum powder and sodium molybdate powder are added described in step one mix homogeneously in binding agent,
To slurry；The addition of described sodium molybdate powder is according to the matter of sodium in sodium molybdate doped molybdenum to be prepared
Amount percentage composition conversion obtains；3kg is added during the addition of molybdenum powder is every liter of binding agent in the present embodiment
Molybdenum powder, in the present embodiment sodium molybdate to be prepared doped molybdenum, the weight/mass percentage composition of sodium is 3%,
Thus conversing, the addition of sodium molybdate powder is addition 547g sodium molybdate powder in every liter of binding agent；
Step 3, utilize spray drying tower that slurry described in step 2 is carried out spray drying treatment,
To pellet；The intake air temperature controlling spray drying tower during spray drying treatment is 220 DEG C, goes out
Draught temperature is 130 DEG C, and controlling the rotating speed of nebulizer in spray drying tower is 1.1 × 104r/min；
Step 4, under the protection of hydrogen atmosphere, be 650 DEG C by pellet described in step 3 in temperature
Under conditions of be incubated 2h carry out carbonization treatment, obtain sodium molybdate doped molybdenum after natural cooling.
In sodium molybdate doped molybdenum prepared by the present embodiment, the weight/mass percentage composition actual measurement of sodium is 3%, carbon
Mass content be not higher than 50ppm.The metallographic structure of sodium molybdate doped molybdenum prepared by the present embodiment is such as
Shown in Fig. 1, the sodium molybdate doped molybdenum Oxygen potential that as shown in Figure 1 prepared by the present embodiment is high, and size is equal
Even, good product consistency, the requirement to powder of the special forming mode can be met completely.
Embodiment 2
The preparation method of the present embodiment sodium molybdate doped molybdenum comprises the following steps:
Step one, polyacrylamide is added in deionized water it is sufficiently stirred for, until polyacrylamide is complete
CL, obtains binding agent；The addition of described polyacrylamide is addition 3g in every liter of deionized water
Polyacrylamide；
Step 2, molybdenum powder and sodium molybdate powder are added described in step one mix homogeneously in binding agent,
To slurry；The addition of described sodium molybdate powder is according to the matter of sodium in sodium molybdate doped molybdenum to be prepared
Amount percentage composition conversion obtains；2kg is added during the addition of molybdenum powder is every liter of binding agent in the present embodiment
Molybdenum powder, in the present embodiment sodium molybdate to be prepared doped molybdenum, the weight/mass percentage composition of sodium is 1%,
Thus conversing, the addition of sodium molybdate powder is addition 110g sodium molybdate powder in every liter of binding agent；
Step 3, utilize spray drying tower that slurry described in step 2 is carried out spray drying treatment,
To pellet；The intake air temperature controlling spray drying tower during spray drying treatment is 200 DEG C, goes out
Draught temperature is 110 DEG C, and controlling the rotating speed of nebulizer in spray drying tower is 1.0 × 104r/min；
Step 4, under the protection of hydrogen atmosphere, be 700 DEG C by pellet described in step 3 in temperature
Under conditions of be incubated 1.5h carry out carbonization treatment, obtain sodium molybdate doped molybdenum after natural cooling.
In sodium molybdate doped molybdenum prepared by the present embodiment, the weight/mass percentage composition actual measurement of sodium is 1%, carbon
Mass content be not higher than 50ppm.The metallographic structure of sodium molybdate doped molybdenum prepared by the present embodiment is such as
Shown in Fig. 2, the sodium molybdate doped molybdenum Oxygen potential that as shown in Figure 2 prepared by the present embodiment is high, and size is equal
Even, good product consistency, the requirement to powder of the special forming mode can be met completely.
Embodiment 3
The preparation method of the present embodiment sodium molybdate doped molybdenum comprises the following steps:
Step one, polyacrylamide is added in deionized water it is sufficiently stirred for, until polyacrylamide is complete
CL, obtains binding agent；The addition of described polyacrylamide is addition 5g in every liter of deionized water
Polyacrylamide；
Step 2, molybdenum powder and sodium molybdate powder are added described in step one mix homogeneously in binding agent,
To slurry；The addition of described sodium molybdate powder is according to the matter of sodium in sodium molybdate doped molybdenum to be prepared
Amount percentage composition conversion obtains；4kg is added during the addition of molybdenum powder is every liter of binding agent in the present embodiment
Molybdenum powder, in the present embodiment sodium molybdate to be prepared doped molybdenum, the weight/mass percentage composition of sodium is 5%,
Thus conversing, the addition of sodium molybdate powder is addition 1356g sodium molybdate powder in every liter of binding agent；
Step 3, utilize spray drying tower that slurry described in step 2 is carried out spray drying treatment,
To pellet；The intake air temperature controlling spray drying tower during spray drying treatment is 240 DEG C, goes out
Draught temperature is 150 DEG C, and controlling the rotating speed of nebulizer in spray drying tower is 1.3 × 104r/min；
Step 4, under the protection of hydrogen atmosphere, be 600 DEG C by pellet described in step 3 in temperature
Under conditions of be incubated 2.5h carry out carbonization treatment, obtain sodium molybdate doped molybdenum after natural cooling.
In sodium molybdate doped molybdenum prepared by the present embodiment, the weight/mass percentage composition actual measurement of sodium is 5%, carbon
Mass content be not higher than 50ppm.The metallographic structure of sodium molybdate doped molybdenum prepared by the present embodiment is such as
Shown in Fig. 3, the sodium molybdate doped molybdenum Oxygen potential that as shown in Figure 3 prepared by the present embodiment is high, and size is equal
Even, good product consistency, the requirement to powder of the special forming mode can be met completely.
For the checking type for adhesive impact on sodium molybdate doped molybdenum system, the present invention is respectively by equivalent
Polyacrylamide, hydroxypropyl cellulose, carboxymethyl cellulose, Polyethylene Glycol and soluble starch add
Entering and be configured to different types of binding agent in deionized water, the performance comparison of various binding agents is shown in Table 1.
The performance comparison of the various binding agent of table 1
As it can be seen from table 1 whether mix from solution colour and sodium molybdate aqueous solution, viscosity size
Seeing etc. combination property, in five kinds of caking property materials, polyacrylamide adulterates for sodium molybdate of the present invention
Molybdenum powder system, its combination property is optimal, and therefore the present invention finally selectes polyacrylamide is binding agent,
And from usage amount, needed for reaching same viscosity, addition is minimum, this is for removing after pelletize
Carbon in Organic substance is highly advantageous.
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the present invention.All
It is that any simple modification, change and the equivalence made above example according to inventive technique essence becomes
Change, all still fall within the protection domain of technical solution of the present invention.
Claims (2)
1. the preparation method of a sodium molybdate doped molybdenum, it is characterised in that the method includes following
Step:
Step one, polyacrylamide is added in deionized water it is sufficiently stirred for, until polyacrylamide is complete
CL, obtains binding agent；The addition of described polyacrylamide is to add in every liter of deionized water
3g～5g polyacrylamide；
Step 2, molybdenum powder and sodium molybdate powder are added described in step one mix homogeneously in binding agent,
To slurry；The addition of described molybdenum powder is addition 2kg～4kg molybdenum powder, described molybdic acid in every liter of binding agent
The addition of sodium powder is according to the weight/mass percentage composition conversion of sodium in sodium molybdate doped molybdenum to be prepared
Obtain；
Step 3, utilize spray drying tower that slurry described in step 2 is carried out spray drying treatment,
To pellet；The concrete technology parameter of described spray drying treatment is: the intake air temperature of spray drying tower
Being 200 DEG C～240 DEG C, air outlet temperature is 110 DEG C～150 DEG C, and in spray drying tower, nebulizer turns
Speed is 1.0 × 104R/min～1.3 × 104r/min；
Step 4, under the protection of hydrogen atmosphere, by pellet described in step 3 in temperature be
It is incubated 1.5h～2.5h under conditions of 600 DEG C～700 DEG C and carries out carbonization treatment, after natural cooling, obtain molybdic acid
Natrium doping molybdenum powder；In described sodium molybdate doped molybdenum, the weight/mass percentage composition of sodium is 1%～5%, carbon
Mass content is not higher than 50ppm.
The preparation method of a kind of sodium molybdate doped molybdenum the most according to claim 1, its feature
Being, the concrete technology parameter of spray drying treatment described in step 3 is: the air intake of spray drying tower
Mouth temperature is 220 DEG C, and air outlet temperature is 130 DEG C, and in spray drying tower, the rotating speed of nebulizer is
1.1×104r/min。
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| AU2003292731A1 (en) * | 2003-01-08 | 2004-08-10 | Toudaitlo, Ltd. | Magnesium composite powder, method for producing same, magnesium base composite material and method for producing same |
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