CN102294490A - Crude molybdenum powder preparing method - Google Patents
Crude molybdenum powder preparing method Download PDFInfo
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Abstract
The invention discloses a crude molybdenum powder preparing method, which comprises the following steps: mixing molybdenum powder and molybdenum oxide powder according to the weight ratio of (4-0.67):1, then spraying deionized water into the mixed powder according to the proportion of (4ml-8ml)/100g mixed powder, and mixing for 30-60min after stirring uniformly; pressing the mixture into blanks by isostatic pressing; crushing the pressed blanks and then screening to obtain (-20 meshes, 180 meshes) prefabricated powder; carrying out hydrogen reduction on the prefabricated powder, wherein the reduction temperature is 750-970 DEG C, the reduction time is 10-12h, and the hydrogen flow is 20-30L/h; and after ball-milling the prepared molybdenum powder for 30-60min according to the ball material volume ratio of 1.1-2.0, screening to obtain needed products. The method disclosed by the invention has low production cost and a simple process, and the prepared molybdenum powder has a good use performance.
Description
Technical field
The present invention relates to a kind of preparation method of molybdenum, particularly a kind of preliminary compression granulation is produced the method for coarse granule molybdenum powder.
Background technology
As everyone knows, except that the minority noble metal, metal material can be with surrounding medium generation chemical reaction and electrochemical reaction and is corroded.In addition, the metal surface is subjected to various mechanisms and the wearing and tearing that cause are also very serious.Therefore, development protecting metallic surface and reinforcement technique are the key subjects that various countries generally are concerned about.Molybdenum is hindered performance etc. with its good wearability, corrosion resistance and tension and is widely used in the Hyundai Motor industry.Directly adopt molybdenum to make this type component and cost an arm and a leg, and the preparation molybdenum is a coating on the engineering material surface, has both satisfied performance requirement, has reduced cost again.In the automobile industry development process, there is the coating of many models to be used to improve the anti-wear performance of speed changer synchronous ring, internal-combustion engine piston ring, molybdenum is that coating is exactly one of coating that is widely used.Molybdenum is that the preparation of coating is continued to use the method for flame-spraying in China part enterprise always.Molybdenum filament flame-spraying equipment is simple, differs but deposit a size, and oxidization burning loss is serious, and coating is loosened and because of molybdenum filament processes Ben Gaoang, seriously restricted its extensive use.In recent years, make the plasma spraying method of raw material along with the improvement of the automatic doubler surface glouer of disputing, dusty spray production technology is promoted with molybdenum powder.The molybdenum powder cost only is about 50% of a molybdenum filament, for satisfying different performance requirements, can add various alloying elements easily in molybdenum powder, to form desired coating.
The process characteristic of plasma spraying molybdenum coating requires coating molybdenum powder granularity thick (surpassing 10 μ m), suitable particle size distribution and good flowability is arranged.Common molybdenum powder granularity is less and distribute wide, mobile poorly, can not satisfy plasma spray coating process and coating performance requirement.Simultaneously, possess specific performance properties, also must carry out strictness control the chemical composition of coating molybdenum powder for making coating, will be as impurity such as the oxygen in the molybdenum powder, carbon, nitrogen contents to lifting effects such as the hardness of coating, wearabilities.
Influence the technological factor of molybdenum powder granularity, can represent with the following relationship formula:
d＝f(T，ΔT，h，Q，t)
In the formula; D is a powder size; T is a reduction temperature; Δ T is a thermograde; H is a thickness of feed layer in the boat; Q is a hydrogen flowing quantity; T is the recovery time.
Reduction temperature is high more, the molybdenum powder granularity is big more, thickness of feed layer is big more, hydrogen infiltrates and steam is overflowed will be difficult more, in fact be equivalent to increase the dividing potential drop of steam, promote that the molybdenum powder volatilization---deposition is grown up, and makes the particle chap; Hydrogen flowing quantity is big more, and steam is overflowed and speeded up, and then the molybdenum powder granularity is thin more.Recovery time is long, and the molybdenum powder probability that OR is grown up repeatedly, collective recrystallization is grown up is just big, and the molybdenum powder particle is just big more.
The contribution that above-mentioned technological factor is grown up to the molybdenum powder particle is limited, and especially granularity is to obtain with aforesaid way greater than the molybdenum powder of 20 μ m.
At present, in order to adapt to the process characteristic requirement of plasma spraying molybdenum coating, mainly adopt following two kinds of methods to prepare molybdenum powder:
First method is the high temperature sintering fragmentation:
(1) selects suitable conventional molybdenum powder.The granularity and the density of molybdenum powder are moderate, and chemical composition is even, qualified, and the molybdenum powder pattern is rule comparatively, no too much overlap joint.
(2) pressed compact moulding.Adopt the hydraulic press and the mould of enough tonnages, molybdenum powder is pressed into base.
(3) sintering.Select 800 ℃-1200 ℃ temperature, the molybdenum base of compacting is put into sintering furnace sintering 1-5h.
(4) broken and screening.Adopt the method for Mechanical Crushing will carry out fragmentation and screening through the blank of oversintering.
Above-mentioned first method because of sintering after blank harder, Mechanical Crushing need increase the special equipment input, the equipment input is bigger, the production cost height; Prepared powder causes impurity content higher because of pulverizing process, and granule-morphology is irregular, and the flow of powder performance is relatively 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 purifying aquation slurry are mixed with the molybdenum powder material;
(2) the molybdenum powder slip with preparation carries out spray drying granulation;
(3) the molybdenum powder particle that obtains carries out binder removal, sieves, high temperature sintering;
(4) will obtain coating molybdenum powder behind the sieve classification excessively through molybdenum powder ball milling in efficient ball mill of high temperature sintering.
Above-mentioned second method production process complexity wants configure dedicated equipment to increase investment, production cost height; Materials such as PEG that adds in the process of sizing mixing and PVA, impurity such as the carbon that decomposites in the sintering process, oxygen are difficult to eliminate, and influence the serviceability of powder; Material hardness behind the high temperature sintering is big, and ball milling expects to increase the impurity in the thick molybdenum powder firmly.
Summary of the invention
The objective of the invention is at the method production cost height, the complex process that prepare molybdenum powder in the prior art, the problem that the molybdenum powder serviceability is not good provides a kind of method of 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, with common molybdenum powder and molybdenum oxide (MoO
3Or MoO
2) powder is by weight (4～0.67): 1 ratio is mixed, particularly (4～1.5): after 1 ratio is mixed, the ratio of adding 4ml～8ml deionized water according to per 100 gram mixed-powders is sprayed deionized water in mixed-powder again, mixes 30min～60min after stirring again;
B, the static pressure such as mixture employing that steps A is obtained are pressed into base;
C, the compacting base of gained among the step B screened after fragmentation obtain (20 orders ,+180 orders) prefabricated powder;
D, the prefabricated powder of gained among the step C is carried out hydrogen reducing, reduction temperature is 750 ℃～970 ℃; Recovery time is 10h～12h, hydrogen flowing quantity: 20L/h～30L/h;
E, the powder material of gained among the step D is sent into ball mill, add agate ball in the ball mill, ball material volume ratio is 1.1～2.0, and behind ball milling 30min～60min, screening obtains required product.
As optimal way, among the described step B, waiting the force value of static pressure compacting is 80MPa～100MPa, and the dwell time is 100s～120s.
As optimal way, among the described step C, after the screening ,+20 purpose oversizes return and continue brokenly, and-180 purpose screenings return and wait static pressure to suppress.
As optimal way, in the described steps A, the Fisher particle size of common molybdenum powder is 2.1 μ m～3.5 μ m, and loose specific weight is 0.8g/cm
3～1.1g/cm
3
MoO
2The Fisher particle size of powder is 5.0 μ m～7.0 μ m, and loose specific weight is 0.6g/cm
3～1.2g/cm
3
MoO
3The Fisher particle size of powder is 5.7 μ m～7.8 μ m, and loose specific weight is 0.7g/cm
3～1.2g/cm
3
The inventive method is a raw material with molybdenum powder and molybdenum oxide powder,, as the lubricant between molybdenum powder and the molybdenum oxide particle three is mixed with water, carries out pre-stampedly in equal pressing equipment, obtains the precompressed blank with certain intensity.Blank, is chosen the powder of (20 orders ,+180 orders) prefabricated grain according to the requirement of user to thick molybdenum powder after appropriateness fragmentation, screening, the thick molybdenum powder of the mistake that exceeds particle size range is carried out ball-milling treatment, and the raw material that meticulous molybdenum powder be can be used as preliminary compression granulation is reused.In the condition and range that existing molybdenum powder reduction equipment allows, in hydrogen atmosphere, be reduced into molybdenum powder, molybdenum powder is through sieve classification, can produce the thick molybdenum powder that satisfies customer requirements (for example the granularity Fisher particle size surpasses 10 μ m, even up to the bulky grain molybdenum powder about 20 μ m).
In technical solution of the present invention, add molybdenum powder as molybdenum oxide (as MoO
3) volatilize during powder reduction---the core that deposition is grown up, by the difference of two kinds of material thermodynamic properties, thus accelerating oxidation---carrying out repeatedly of reduction reaction.Though MoO
3Particle and Mo powder particles contact area have the generation of intermidate oxide, but MoO
3Particle and Mo particle contact area are always to MoO
3The side migration, the Mo aggregate is grown up.Add deionized water, as the lubricant between molybdenum powder and the molybdenum trioxide particle, help being pressed in advance base during precompressed; During hydrogen reducing, increased the dividing potential drop of steam, quickened the migration that molybdenum powder and molybdenum trioxide interfacial reaction generate molybdenum powder, promoted that the volatilization of molybdenum powder particle---deposition is grown up, helped powder particle and reunite closely.Therefore, add a certain amount of MoO in the molybdenum powder
3, carry out " humidification " prefabricated grain again after, handle by hydrogen heat, can obtain thick molybdenum powder.
Thereby the inventive method has been avoided because of Mechanical Crushing or has been added the impurity content that binding agent increases made molybdenum powder, and it is low to prepare impurity content, the coarse granule molybdenum powder that granularity is bigger.The broken method for preparing thick molybdenum powder had reduced preparation difficulty and production cost after this method was compared presintering, had simplified preparation process.By an amount of molybdenum oxide and deionized water (because the exchange of adding in the molybdenum powder of the gas in the reduction process, if molybdenum oxide adds and too much will cause the made powder particle group loose), in hydrogen reducing and sintering process, help improving the intensity of molybdenum powder aggregate.The powder size of preparing by the inventive method is more than 10 μ m, even up to about 20 μ m, loose specific weight is greater than 1.5g/cm
3
Description of drawings
Fig. 1 is a process chart of the present invention.
The specific embodiment
Disclosed all features in this specification, or the step in disclosed all methods or the process except mutually exclusive feature and/or step, all can make up by any way.
Embodiment 1: as shown in Figure 1, a kind of method of producing the coarse granule molybdenum powder comprises the steps:
A, with common molybdenum powder: MoO
3Powder sprays deionized water according to the ratio of 4ml deionized water/100g mixed-powder after mixing by weight 1.5: 1 ratios in mixed-powder, mix 60min after stirring again;
B, the static pressure such as mixture employing of steps A are pressed into base, waiting the force value of static pressure compacting is 100MPa, and the dwell time is 100s;
C, the compacting base of gained among the step B screened after fragmentation obtain (20 orders ,+180 orders) prefabricated powder; After the screening ,+20 purpose oversizes return and continue brokenly, and-180 purpose screenings return and wait static pressure to suppress.
D, the prefabricated powder of gained among the step C is carried out hydrogen reducing, reduction temperature is 750 ℃; Recovery time is 12h, hydrogen flowing quantity: 20L/h;
E, the powder material of gained among the step D is sent into ball mill, the agate ball in the ball mill and the volume ratio of compound are 2.0: 1, and behind made molybdenum powder ball milling 30min, it is 14.5 μ m that screening obtains the required product Fisher particle size, and loose specific weight is 1.90g/cm
3
Embodiment 2: as shown in Figure 1, a kind of method of producing the coarse granule molybdenum powder comprises the steps:
A, with common molybdenum powder and MoO
2Powder sprays deionized water according to the ratio of 8ml deionized water/100g mixed-powder after mixing by weight 4: 1 in mixed-powder, mix 30min after stirring again;
B, the static pressure such as mixture employing of steps A are pressed into base, waiting the force value of static pressure compacting is 100MPa, and the dwell time is 114s;
C, the compacting base of gained among the step B screened after fragmentation obtain (20 orders ,+180 orders) prefabricated powder; After the screening ,+20 purpose oversizes return and continue brokenly, and-180 purpose screenings return and wait static pressure to suppress.
D, the prefabricated powder of gained among the step C is carried out hydrogen reducing, reduction temperature is 970 ℃; Recovery time is 10h, hydrogen flowing quantity: 20L/h;
E, the powder material of gained among the step D is sent into ball mill, add agate ball in ball mill, ball material volume ratio is 1.5: 1, and behind made molybdenum powder ball milling 60min, it is 15.2 μ m that screening obtains the required product Fisher particle size, and loose specific weight is 2.13g/cm
3
Embodiment 3: a kind of method of producing the coarse granule molybdenum powder comprises the steps:
A, with common molybdenum powder: MoO
3Powder sprays deionized water according to the ratio of 8ml deionized water/100g mixed-powder after mixing by weight 4: 1 ratios in mixed-powder, mix 30min after stirring again;
B, the static pressure such as mixture employing of steps A are pressed into base, waiting the force value of static pressure compacting is 100MPa, and the dwell time is 114s;
C, the compacting base of gained among the step B screened after fragmentation obtain (20 orders ,+180 orders) prefabricated powder; After the screening ,+20 purpose oversizes return and continue brokenly, and-180 purpose screenings return and wait static pressure to suppress.
D, the prefabricated powder of gained among the step C is carried out hydrogen reducing, reduction temperature is 970 ℃; Recovery time is 12h, hydrogen flowing quantity: 20L/h;
E, the powder material of gained among the step D is sent into ball mill, the volume ratio of agate ball in the ball mill and powder material is 1.5: 1, and behind made molybdenum powder ball milling 30min, it is 22.0 μ m that screening obtains the required product Fisher particle size, and loose specific weight is 2.23g/cm
3
Embodiment 4: a kind of method of producing the coarse granule molybdenum powder comprises the steps:
A, with common molybdenum powder: MoO
3Powder sprays deionized water according to the ratio of 6ml deionized water/100g mixed-powder after mixing by weight 0.67: 1 ratio in mixed-powder, mix 40min after stirring again;
B, the static pressure such as mixture employing of steps A are pressed into base, waiting the force value of static pressure compacting is 80MPa, and the dwell time is 120s;
C, the compacting base of gained among the step B screened after fragmentation obtain (20 orders ,+180 orders) prefabricated powder; After the screening ,+20 purpose oversizes return and continue brokenly, and-180 purpose screenings return and wait static pressure to suppress.
D, the prefabricated powder of gained among the step C is carried out hydrogen reducing, reduction temperature is 970 ℃; Recovery time is 12h, hydrogen flowing quantity: 30L/h;
E, the powder material of gained among the step D is sent into ball mill, the volume ratio of agate ball in the ball mill and powder material is 1.1: 1, and behind made molybdenum powder ball milling 30min, it is 13.4 μ m that screening obtains the required product Fisher particle size, and loose specific weight is 1.78g/cm
3
Among above-mentioned four embodiment, the Fisher particle size of common molybdenum powder is 2.1 μ m～3.5 μ m, and loose specific weight is 0.8g/cm
3～1.1g/cm
3MoO
2The Fisher particle size of powder is 5.0 μ m～7.0 μ m, and loose specific weight is 0.6g/cm
3～1.2g/cm
3MoO
3The Fisher particle size of powder is 5.7 μ m～7.8 μ m, and loose specific weight is 0.7g/cm
3～1.2g/cm
3In the foregoing description, the used agate ball of ball milling also can adopt steel ball to grind as required.
The inventive method production cost of employing the foregoing description is low, technology is simple, and prepared molybdenum powder serviceability is good.
The present invention is not limited to the aforesaid specific embodiment.The present invention expands to any new feature or any new combination that discloses in this manual, and the arbitrary new method that discloses or step or any new combination of process.
Claims (6)
1. a method of producing thick molybdenum powder is characterized in that comprising the steps:
A, with common molybdenum powder: the molybdenum oxide powder is by weight (4～0.67): after 1 ratio is mixed, restrain the ratio that mixed-powders add 4ml～8ml deionized waters according to per 100 again, in above-mentioned mixed-powder, spray deionized water, mix 30min～60min after stirring again;
B, mixture that steps A is obtained through etc. static pressure be pressed into base;
C, the compacting base that step B is obtained screen after fragmentation, obtain the prefabricated grain powder of powder size for (20 orders ,+180 orders);
D, the prefabricated grain powder that is obtained among the step C is carried out hydrogen reducing, reduction temperature is 750 ℃～970 ℃; Recovery time is 10h～12h, hydrogen flowing quantity: 20L/h～30L/h;
E, the powder material that step D is obtained are sent into ball mill, add agate ball or steel ball in ball mill, and ball material volume ratio be (1.1～2.0): 1, and behind ball milling 30min～60min, sieve and obtain required thick molybdenum powder.
2. the method for producing thick molybdenum powder as claimed in claim 1 is characterized in that: described steps A replaces with following steps:
A ', with common molybdenum powder: the molybdenum oxide powder is by weight (4～1.5): after 1 ratio is mixed, restrain the ratio that mixed-powders add 4ml～8ml deionized waters according to per 100 again, in above-mentioned mixed-powder, spray deionized water, mix 30min～60min after stirring again.
3. the method for producing thick molybdenum powder as claimed in claim 1 or 2 is characterized in that: described molybdenum oxide is MoO
3Or MoO
2
4. the method for producing thick molybdenum powder as claimed in claim 1 or 2 is characterized in that: among the described step B, waiting the force value of static pressure compacting is 80MPa～100MPa, and the dwell time is 100s～120s.
5. the method for producing thick molybdenum powder as claimed in claim 1 or 2 is characterized in that: among the described step C, after the screening ,+20 purpose oversizes return and continue brokenly, and-180 purpose screenings return and wait static pressure to suppress.
6. the method for producing thick molybdenum powder as claimed in claim 1 or 2 is characterized in that:
The Fisher particle size of described common molybdenum powder is 2.1 μ m～3.5 μ m, and loose specific weight is 0.8g/cm
3～1.1g/cm
3
MoO
2The Fisher particle size of powder is 5.0 μ m～7.0 μ m, and loose specific weight is 0.6g/cm
3～1.2g/cm
3
MoO
3The Fisher particle size of powder is 5.7 μ m～7.8 μ m, and loose specific weight is 0.7g/cm
3～1.2g/cm
3
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Cited By (6)
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| CN103276271A (en) * | 2013-05-07 | 2013-09-04 | 常州市茂盛特合金制品有限公司 | High-purity high-activity molybdenum ball and preparation method |
| CN104439266A (en) * | 2014-12-12 | 2015-03-25 | 金堆城钼业股份有限公司 | Preparation method of molybdenum powder large in particle size |
| CN104445407A (en) * | 2014-12-10 | 2015-03-25 | 九江有色金属冶炼有限公司 | Preparation method of granular niobium oxide and granular niobium oxide prepared by same |
| CN106041104A (en) * | 2016-06-23 | 2016-10-26 | 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 |
| CN114833349A (en) * | 2022-07-04 | 2022-08-02 | 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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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103276271A (en) * | 2013-05-07 | 2013-09-04 | 常州市茂盛特合金制品有限公司 | High-purity high-activity molybdenum ball and preparation method |
| CN104445407A (en) * | 2014-12-10 | 2015-03-25 | 九江有色金属冶炼有限公司 | Preparation method of granular niobium oxide and granular niobium oxide prepared by same |
| 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 |
| CN104439266A (en) * | 2014-12-12 | 2015-03-25 | 金堆城钼业股份有限公司 | Preparation method of molybdenum powder large in particle size |
| 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 |
| CN106041104A (en) * | 2016-06-23 | 2016-10-26 | 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 |
| CN114833349A (en) * | 2022-07-04 | 2022-08-02 | 成都虹波实业股份有限公司 | Method for manufacturing low-potassium large-particle-size molybdenum powder |
| 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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