CN102294490B - A kind of method producing thick molybdenum powder - Google Patents
A kind of method producing thick molybdenum powder Download PDFInfo
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Abstract
The invention discloses a kind of method producing thick molybdenum powder, by molybdenum powder: molybdenum oxide powder is (4～0.67) by weight: after the ratio mixing of 1, in mixed-powder, spray deionized water according to the ratio of (4ml～8ml)/100g mixed-powder, after stirring, remix 30min～60min；Isostatic pressed is adopted to be pressed into base in mixture；Compacting base screens after crushing and obtains (-20 orders ,+180 orders) pre-made powder；Pre-made powder carries out hydrogen reducing, and reduction temperature is 750 DEG C～970 DEG C；Recovery time is 10h～12h, hydrogen flowing quantity: 20L/h-30L/h；Being 1.1～2.0 according to ball material volume ratio, after made molybdenum powder ball milling 30min～60min, screening obtains required product.The inventive method production cost is low, technique simple, and prepared molybdenum powder serviceability is good.
Description
Technical field
The preparation method that the present invention relates to a kind of molybdenum powder, particularly to a kind of method of preparing coarse particle molybdenum powder by preliminary compression granulation.
Background technology
It is known that except minority noble metal, metal material can be corroded with surrounding medium generation chemical reaction and electrochemical reaction.Additionally, the abrasion that metal surface is caused by various mechanisms is also extremely serious.Therefore, develop protecting metallic surface and reinforcement technique, be the key subjects of various countries' general concern.Molybdenum is hindered performance etc. with its excellent wearability, corrosion resistance and tension and is widely used in modern automobile industry.Directly adopt molybdenum to manufacture this type component expensive, and on engineering material surface, prepare molybdenum system coating, both met performance requirement, reduced again cost.In automobile industry development process, having the coating of many models to be used to improve the anti-wear performance of variator synchronous ring, internal-combustion engine piston ring, molybdenum system coating is exactly one of coating of being widely used.The method that the preparation of molybdenum system coating continues to use flame-spraying at China's Some Enterprises always.Molybdenum filament flame spray device is simple, but a deposition size differs, and oxidization burning loss is serious, and coating is loose and because molybdenum filament processes high, serious restricts its extensive use.In recent years, make the plasma spraying method of raw material with molybdenum powder and promoted along with the improvement of automatic doubler surface glouer of disputing, dusty spray production technology.Molybdenum powder cost is only about the 50% of molybdenum filament, for meeting different performance requirements, it is convenient to add various alloying element in molybdenum powder, to form desired coating.
The process characteristic of plasma spraying molybdenum coating requires coating molybdenum powder granularity relatively thick (more than 10 μm), has suitable particle size distribution and good mobility.Common molybdenum powder granularity is less and distribution is wide, poor fluidity, it is impossible to meet plasma spray coating process and coating performance requirement., for making coating possess specific performance, must also the chemical composition of coating molybdenum powder strictly being controlled, the impurity such as oxygen in molybdenum powder, carbon, nitrogen content is by lifting effects such as the hardness of coating, wearabilities meanwhile.
Affect the technological factor of molybdenum powder granularity, it is possible to represent by following relationship:
D=f (T, Δ T, h, Q, t)
In formula；D is powder size；T is reduction temperature；Δ T is thermograde；H is thickness of feed layer in boat；Q is hydrogen flowing quantity；T is the recovery time.
Reduction temperature is more high, molybdenum powder granularity is more big, thickness of feed layer is more big, hydrogen penetrates into and steam effusion will be more difficult, is effectively equivalent to add the dividing potential drop of steam, promotes that molybdenum powder volatilization deposition is grown up, makes granule thicker；Hydrogen flowing quantity is more big, and steam effusion speed is accelerated, then molybdenum powder granularity is more thin.Recovery time is long, and the probability that molybdenum powder oxidation-reduction repeatedly is grown up, collective recrystallization is grown up is just big, and molybdenum powder granule is more big.
The contribution of molybdenum powder particle growth is limited by above-mentioned technological factor, and especially the granularity molybdenum powder more than 20 μm is to obtain in fashion described above.
At present, in order to adapt to the process characteristic requirement of plasma spraying molybdenum coating, main employing following two method prepares molybdenum powder:
First method is that high temperature sintering crushes:
(1) suitable conventional molybdenum powder is selected.The granularity of molybdenum powder and medium density, chemical composition is uniform, qualified, and shape of molybdenum powder is comparatively regular, without too much overlap joint.
(2) pressed compact molding.Adopt hydraulic press and the mould of enough tonnages, molybdenum powder is pressed into base.
(3) sintering.Select the temperature of 800 DEG C-1200 DEG C, the molybdenum base of compacting is put into sintering furnace sintering 1-5h.
(4) crush and sieve.Blank through oversintering is carried out broken and sieves by the method adopting Mechanical Crushing.
Above-mentioned first method because of after sintering blank harder, Mechanical Crushing needs to increase special equipment and puts into, and equipment investment is relatively big, and production cost is high；Because of pulverizing process, prepared powder causes that impurity content is higher, granule-morphology is irregular, and flow of powder performance is poor, has a strong impact on the serviceability of powder.
Second method is that bonding is granulated:
(1) molybdenum powder and PEG, PVA and ethanol and purification aquation slurry are configured to molybdenum powder material；
(2) the molybdenum powder slip of preparation is carried out spray drying granulation；
(3) the molybdenum powder granule obtained carries out binder removal, sieves, high temperature sintering；
(4) by the ball milling in efficient ball mill of the molybdenum powder through high temperature sintering, after crossing sieve classification, coating molybdenum powder is obtained.
Above-mentioned second method production process is complicated, and will configure special equipment increases investment, and production cost is high；The material such as PEG and PVA added in process of sizing mixing, the impurity such as the carbon decomposited in sintering process, oxygen is difficult to eliminate, and affects the serviceability of powder；Material hardness after high temperature sintering is big, and ball milling expects to increase the impurity in thick molybdenum powder firmly.
Summary of the invention
Present invention aims to prior art is prepared the method production cost height of molybdenum powder, complex process, the problem that molybdenum powder serviceability is not good, it is provided that a kind of method producing thick molybdenum powder.
For achieving the above object, the technical solution adopted for the present invention to solve the technical problems is as follows:
A, by common molybdenum powder and molybdenum oxide (MoO3Or MoO2) powder is by weight (4～0.67): the ratio mixing of 1, particularly (4～1.5): after the ratio mixing of 1, the ratio of 4ml～8ml deionized water is added according still further to every 100 grams of mixed-powders, in mixed-powder, spray deionized water, after stirring, remix 30min～60min；
B, by step A obtain mixture adopt isostatic pressed be pressed into base；
C, the compacting base of gained in step B is screened after crushing obtain (-20 orders ,+180 orders) pre-made powder；
D, the pre-made powder of gained in step C being carried out hydrogen reducing, reduction temperature is 750 DEG C～970 DEG C；Recovery time is 10h～12h, hydrogen flowing quantity: 20L/h～30L/h；
E, by step D gained powder materials send into ball mill, in ball mill add agate ball, ball material volume ratio is 1.1～2.0, after ball milling 30min～60min, screening obtain required product.
It is preferred that, in described step B, the force value of isostatic pressed compacting is 80MPa～100MPa, and the dwell time is 100s～120s.
It is preferred that, in described step C, after screening, the oversize of+20 orders returns and continues to crush, and the siftage of-180 orders returns isostatic pressed compacting.
It is preferred that, in described step A, the Fisher particle size of common molybdenum powder is 2.1 μm～3.5 μm, and loose specific weight is 0.8g/cm3～1.1g/cm3；
MoO2The Fisher particle size of powder is 5.0 μm～7.0 μm, and loose specific weight is 0.6g/cm3～1.2g/cm3；
MoO3The Fisher particle size of powder is 5.7 μm～7.8 μm, and loose specific weight is 0.7g/cm3～1.2g/cm3。
The inventive method is with molybdenum powder and molybdenum oxide powder for raw material, using water as the lubricant between molybdenum powder and molybdenum oxide granule, three is mixed, carries out pre-stamped, it is thus achieved that have the precompressed blank of some strength in equal pressing equipment.Blank is broken through appropriateness, after screening, according to user's requirement to thick molybdenum powder, choose the powder of (-20 orders ,+180 orders) prefabricated grain, the thick molybdenum powder of mistake beyond particle size range is carried out ball-milling treatment, meticulous molybdenum powder can be reused as the raw material of preliminary compression granulation.In the condition and range that existing molybdenum powder reduction equipment allows, hydrogen atmosphere is reduced into molybdenum powder, the screened classification of molybdenum powder, it is possible to produce and meet the thick molybdenum powder (such as granularity Fisher particle size more than 10 μm, the bulky grain molybdenum powder even as high as about 20 μm) that user requires.
In technical solution of the present invention, add molybdenum powder as molybdenum oxide (such as MoO3) powder reduction time the volatilization core grown up of deposition, by the difference of two kinds of material thermodynamic properties, thus promoting being repeatedly performed of redox reaction.Although MoO3Granule and Mo powder particles contact area have a generation of intermidate oxide, but MoO3Granule and Mo granule contact area are always to MoO3Side migrates, and Mo aggregate is grown up.Add deionized water, as the lubricant between molybdenum powder and molybdenum trioxide particles during precompressed, be conducive to being pressed in advance base；During hydrogen reducing, increase the dividing potential drop of steam, accelerate the migration of molybdenum powder and molybdenum trioxide interfacial reaction generation molybdenum powder, promote that molybdenum powder granule volatilization deposition is grown up, be conducive to powder particle to reunite closely.Therefore, molybdenum powder adds a certain amount of MoO3, then after carrying out " humidification " prefabricated grain, processed by hydrogen heat, thick molybdenum powder can be obtained.
Inventive process avoids because of Mechanical Crushing or add binding agent thus increasing the impurity content of made molybdenum powder, impurity content can be prepared low, the coarse particle molybdenum powder that granularity is bigger.This method crushes, after comparing presintering, the method preparing thick molybdenum powder and reduces preparation difficulty and production cost, simplifies preparation process.By in molybdenum powder add appropriate molybdenum oxide and deionized water (due to the gas exchange in reduction process, if it is loose that molybdenum oxide interpolation too much may result in made powder particle group), in hydrogen reducing with sintering process, be conducive to improving the intensity of molybdenum powder aggregate.The powder size prepared by the inventive method is more than 10 μm, and even as high as about 20 μm, loose specific weight is more than 1.5g/cm3。
Accompanying drawing explanation
Fig. 1 is present invention process flow chart.
Detailed description of the invention
All features disclosed in this specification, or the step in disclosed all methods or process, except mutually exclusive feature and/or step, all can combine by any way.
Embodiment 1: as it is shown in figure 1, a kind of method producing coarse particle molybdenum powder, comprise the steps:
A, by common molybdenum powder: MoO3Powder is by weight, after 1.5: 1 ratio mixing, spraying deionized water according to the ratio of 4ml deionized water/100g mixed-powder, remix 60min after stirring in mixed-powder；
B, the mixture of step A adopting isostatic pressed be pressed into base, the force value of isostatic pressed compacting is 100MPa, and the dwell time is 100s；
C, the compacting base of gained in step B is screened after crushing obtain (-20 orders ,+180 orders) pre-made powder；After screening, the oversize of+20 orders returns and continues to crush, and the siftage of-180 orders returns isostatic pressed compacting.
D, the pre-made powder of gained in step C being carried out hydrogen reducing, reduction temperature is 750 DEG C；Recovery time is 12h, hydrogen flowing quantity: 20L/h；
E, the powder materials of gained in step D being sent into ball mill, the volume ratio of the agate ball in ball mill and compound is 2.0: 1, and after made molybdenum powder ball milling 30min, it is 14.5 μm that screening obtains required product Fisher particle size, and loose specific weight is 1.90g/cm3。
Embodiment 2: as it is shown in figure 1, a kind of method producing coarse particle molybdenum powder, comprise the steps:
A, by common molybdenum powder and MoO2Powder is by weight, after 4: 1 mixing, spraying deionized water according to the ratio of 8ml deionized water/100g mixed-powder, remix 30min after stirring in mixed-powder；
B, the mixture of step A adopting isostatic pressed be pressed into base, the force value of isostatic pressed compacting is 100MPa, and the dwell time is 114s；
C, the compacting base of gained in step B is screened after crushing obtain (-20 orders ,+180 orders) pre-made powder；After screening, the oversize of+20 orders returns and continues to crush, and the siftage of-180 orders returns isostatic pressed compacting.
D, the pre-made powder of gained in step C being carried out hydrogen reducing, reduction temperature is 970 DEG C；Recovery time is 10h, hydrogen flowing quantity: 20L/h；
E, the powder materials of gained in step D being sent into ball mill, add agate ball in ball mill, ball material volume ratio is 1.5: 1, and after made molybdenum powder ball milling 60min, to obtain required product Fisher particle size be 15.2 μm in screening, and loose specific weight is 2.13g/cm3。
Embodiment 3: a kind of method producing coarse particle molybdenum powder, comprises the steps:
A, by common molybdenum powder: MoO3Powder is by weight, after 4: 1 ratio mixing, spraying deionized water according to the ratio of 8ml deionized water/100g mixed-powder, remix 30min after stirring in mixed-powder；
B, the mixture of step A adopting isostatic pressed be pressed into base, the force value of isostatic pressed compacting is 100MPa, and the dwell time is 114s；
C, the compacting base of gained in step B is screened after crushing obtain (-20 orders ,+180 orders) pre-made powder；After screening, the oversize of+20 orders returns and continues to crush, and the siftage of-180 orders returns isostatic pressed compacting.
D, the pre-made powder of gained in step C being carried out hydrogen reducing, reduction temperature is 970 DEG C；Recovery time is 12h, hydrogen flowing quantity: 20L/h；
E, the powder materials of gained in step D being sent into ball mill, the volume ratio of the agate ball in ball mill and powder materials is 1.5: 1, and after made molybdenum powder ball milling 30min, it is 22.0 μm that screening obtains required product Fisher particle size, and loose specific weight is 2.23g/cm3。
Embodiment 4: a kind of method producing coarse particle molybdenum powder, comprises the steps:
A, by common molybdenum powder: MoO3Powder is by weight, after 0.67: 1 ratio mixing, spraying deionized water according to the ratio of 6ml deionized water/100g mixed-powder, remix 40min after stirring in mixed-powder；
B, the mixture of step A adopting isostatic pressed be pressed into base, the force value of isostatic pressed compacting is 80MPa, and the dwell time is 120s；
C, the compacting base of gained in step B is screened after crushing obtain (-20 orders ,+180 orders) pre-made powder；After screening, the oversize of+20 orders returns and continues to crush, and the siftage of-180 orders returns isostatic pressed compacting.
D, the pre-made powder of gained in step C being carried out hydrogen reducing, reduction temperature is 970 DEG C；Recovery time is 12h, hydrogen flowing quantity: 30L/h；
E, the powder materials of gained in step D being sent into ball mill, the volume ratio of the agate ball in ball mill and powder materials is 1.1: 1, and after made molybdenum powder ball milling 30min, it is 13.4 μm that screening obtains required product Fisher particle size, and loose specific weight is 1.78g/cm3。
In above-mentioned four embodiments, the Fisher particle size of common molybdenum powder is 2.1 μm～3.5 μm, and loose specific weight is 0.8g/cm3～1.1g/cm3；MoO2The Fisher particle size of powder is 5.0 μm～7.0 μm, and loose specific weight is 0.6g/cm3～1.2g/cm3。MoO3The Fisher particle size of powder is 5.7 μm～7.8 μm, and loose specific weight is 0.7g/cm3～1.2g/cm3.In above-described embodiment, the agate ball used by ball milling can also adopt steel ball to be ground as required.
The inventive method production cost of employing above-described embodiment is low, technique simple, and prepared molybdenum powder serviceability is good.
The invention is not limited in aforesaid detailed description of the invention.The present invention expands to any new feature disclosed in this manual or any new combination, and the step of the arbitrary new method disclosed or process or any new combination.
Claims (5)
1. the method producing thick molybdenum powder, it is characterised in that comprise the steps:
A, by common molybdenum powder: molybdenum oxide powder is by weight (4～1.5): after the ratio mixing of 1, the ratio of 4ml～8ml deionized water is added according still further to every 100 grams of mixed-powders, in above-mentioned mixed-powder, spray deionized water, after stirring, remix 30min～60min；
B, by step A obtain mixture be pressed into base through isostatic pressed；
C, the compacting base obtained by step B screen after crushing, obtain the prefabricated grain powder that powder size is-20 order～+180 orders；
D, the prefabricated grain powder obtained in step C being carried out hydrogen reducing, reduction temperature is 750 DEG C～970 DEG C；Recovery time is 10h～12h, hydrogen flowing quantity: 20L/h～30L/h；
E, the powder materials obtained by step D send into ball mill, add agate ball in ball mill, and ball material volume ratio is (1.1～2.0): 1, and after ball milling 30min～60min, screening obtains required thick molybdenum powder.
2. the method producing thick molybdenum powder as claimed in claim 1, it is characterised in that: described molybdenum oxide is MoO3Or MoO2。
3. the method producing thick molybdenum powder as claimed in claim 1, it is characterised in that: in described step B, the force value of isostatic pressed compacting is 80MPa～100MPa, and the dwell time is 100s～120s.
4. the method producing thick molybdenum powder as claimed in claim 1, it is characterised in that: in described step C, after screening, the oversize of+20 orders returns and continues to crush, and the siftage of-180 orders returns isostatic pressed compacting.
5. the method producing thick molybdenum powder as claimed in claim 2, it is characterised in that:
The Fisher particle size of described common molybdenum powder is 2.1 μm～3.5 μm, and loose specific weight is 0.8g/cm3～1.1g/cm3；
MoO2The Fisher particle size of powder is 5.0 μm～7.0 μm, and loose specific weight is 0.6g/cm3～1.2g/cm3；
MoO3The Fisher particle size of powder is 5.7 μm～7.8 μm, and loose specific weight is 0.7g/cm3～1.2g/cm3。
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| CN103276271B (en) * | 2013-05-07 | 2015-03-11 | 常州市茂盛特合金制品有限公司 | High-purity high-activity molybdenum ball and preparation method |
| CN104445407B (en) * | 2014-12-10 | 2016-07-20 | 九江有色金属冶炼有限公司 | The preparation method of a kind of granular niobium oxide and the granular niobium oxide of preparation thereof |
| CN104439266B (en) * | 2014-12-12 | 2016-07-06 | 金堆城钼业股份有限公司 | A kind of preparation method of big particle size molybdenum powder |
| CN106041104B (en) * | 2016-06-23 | 2018-09-21 | 青岛理工大学 | Preparation method for coarsening fine metal powder |
| CN114713834A (en) * | 2022-03-09 | 2022-07-08 | 自贡硬质合金有限责任公司 | High-purity molybdenum powder for sputtering target and preparation method thereof |
| CN114833349B (en) * | 2022-07-04 | 2023-01-31 | 成都虹波实业股份有限公司 | Method for manufacturing low-potassium large-particle-size molybdenum powder |
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