CN101786160B - Special molybdenum powder used for automatic forming and preparation method thereof - Google Patents
Special molybdenum powder used for automatic forming and preparation method thereof Download PDFInfo
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- CN101786160B CN101786160B CN2010103007447A CN201010300744A CN101786160B CN 101786160 B CN101786160 B CN 101786160B CN 2010103007447 A CN2010103007447 A CN 2010103007447A CN 201010300744 A CN201010300744 A CN 201010300744A CN 101786160 B CN101786160 B CN 101786160B
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Abstract
The invention discloses a special molybdenum powder which is directly used for the automatic forming of precision devices of the machinery industry and the electronic industry. The invention is characterized in that the molybdenum powder comprises the following materials according to the parts by mass: 96.6-99.5 parts of primary molybdenum powder, 0.5-2.4 parts of polyvinyl alcohol, 0-0.4 part of polyethylene glycol, 0-0.5 part of metallic stearate and 0-0.15 part of ammonium polyacrylate. The molybdenum powder has good flowability, high apparent density and appropriate particle size distribution and has the self-lubricating action in the process of the automatic forming. The invention also discloses a preparation method of the special molybdenum powder, which comprises the processes: (1) forming agent solution is prepared by the polyvinyl alcohol, the polyethylene glycol, water and other additives; (2) wet grinding is carried out on the primary molybdenum powder, metallic balls and the forming agent solution by proportion in a ball milling tank to prepare molybdenum powder slurry; (3) spray drying is carried out on the prepared molybdenum powder slurry for granulation; (4) the prepared molybdenum powder is collected by a vibrating screen arranged at the discharge hole of a spray drying tower. The preparation method has the greatest advantages of the special molybdenum powder used for the automatic forming can be prepared by one step, the efficiency is high, the cost is low, and the industrialization and no pollution can be realized.
Description
Technical field
A kind of special molybdenum powder that adopts one-step method preparation relates to and a kind ofly is used for machinery, electron trade accurate device automatic extruding is shaped with special molybdenum powder and preparation method thereof.
Background technology
Powder metallurgy is the effective ways of producing the precision metallic device in machinery, electron trade, and its advantage is that the device of producing is wear-resisting, durable, precision is high, noise is little, is applicable to the spare and accessory parts that different shape is complicated, machined is difficult.Simultaneously also can practice thrift metal material, reduce the cut amount, raise labour productivity, save producing cost, reduce production costs, improve the production competitiveness.Full-automatic die forming is a kind of typical shaping means of powder metallurgy, and this method is had relatively high expectations to granularity, flowability and the size distribution of powder.The metal dust of mobile difference can not be used for automatic extruding production, even manually fill mould, if die cavity is complicated, then still even loading mould cavity of powder causes the low and skewness of green density.Obtain having the powder of good compaction performance, generally need initial powder is handled, to improve its granularity and size distribution mobile and acquisition is suitable.Low-melting-point metal can change its granularity, sphericity and size distribution through Technology for Heating Processing, and refractory metal then is difficult for accomplishing.Conventional reduction molybdenum powder granule-morphology is irregular, and powder particle size is less, usually less than 10 μ, does not have flowability, can't realize automatic compacting.And that the reduction molybdenum powder of large scale prepares difficulty is bigger, and will reduce sintering power greatly, thereby is unfavorable for the compaction process and the energy-saving and emission-reduction of goods sintering.All be through multistep processes usually in research in the past; Be about to initial molybdenum powder at a certain temperature after the sintering; Method through broken ball milling or plasma spheroidization prepares the molybdenum powder with high apparent density and flowability; Complex steps, the production efficiency of these methods is low, equipment cost is high, if be used for the greasy property of automatic extruding shaping also need the improvement through other means powder.
The spraying granulation technology is a kind of more advanced disposable granulating technique, and it is based upon on the spray drying technology basis.Spray-drying is to make liquid material get into the process that changes dry powder in the hot drying medium into through spraying; Only limit to minority products such as powdered egg, milk powder during beginning; Along with the research and development that deepens continuously, extensive use in commercial production such as chemistry, food, medicine, agricultural chemicals, pottery, cement, aquatic products, forestry, metallurgy at present.The present invention is to use spray drying technology to carry out the preparation of automatic extruding shaping with molybdenum powder, and this method realizes the special molybdenum powder of step preparation high fluidity and apparent density.
Summary of the invention
The purpose of this invention is to provide the special molybdenum powder that a kind of automatic forming is used.
Another object of the present invention provides the method for the above-mentioned automatic forming of preparation with special molybdenum powder.
A kind of automatic forming of the present invention is used special molybdenum powder; Consisting of of this special molybdenum powder: the mass fraction of raw material molybdenum powder is 96.6～99.5; The mass fraction of polyvinyl alcohol is 0.5～2.4; The mass fraction of polyethylene glycol is 0～0.4, and the mass fraction of Metallic stearates is for being 0～0.5, and the mass fraction of ammonium polyacrylate is 0～0.15.
Above-mentioned special molybdenum powder provided by the invention is realized through following technical scheme.
A kind of automatic forming provided by the invention is with the preparation method of special molybdenum powder, and its preparation process is:
(1) the binder solution of preparation polyvinyl alcohol, polyethylene glycol, water and other additives.
(2) raw material molybdenum powder, Metal Ball and above-mentioned binder solution are carried out wet-milling in proportion in ball grinder and be mixed with the molybdenum powder slip.
(3) the molybdenum powder slip with preparation carries out spray-drying process.
(4) molybdenum powder that makes is collected through spray drying tower discharging opening vibratory sieve.
A kind of automatic forming provided by the invention is with the preparation method of special molybdenum powder, and the process for preparation of described binder solution is that at first weight to be that 0～5 part of Metallic stearates is dissolved into the ethanolic solution of preparation Metallic stearates in 10 parts of ethanol subsequent use.Be 200～500 parts pure water then with weight; 5～25 parts polyvinyl alcohol; 0～4 part polyethylene glycol stirs fully dissolving in 2 hours under 80～90 ℃ temperature; The cooling back adds the ethanolic solution of the Metallic stearates of preparation, and 0～2 part polyacrylic acid ammonium salt solution fully stirs and was modulated into binder solution in 1 hour.
A kind of automatic forming provided by the invention is with the preparation method of special molybdenum powder; The preparation process of molybdenum powder slip is with the raw material molybdenum powder, for the Metal Ball of raw material molybdenum powder weight 100%～300%, puts into the roller ball grinding machine for the above-mentioned binder solution of raw material molybdenum powder weight 20.5～54.6% and carry out wet-milling and mix, and the wet-milling time is 10～36 hours.
A kind of automatic forming provided by the invention is with the preparation method of special molybdenum powder, and what its spray-drying process process adopted is spray drying tower, and the intake air temperature of spray drying tower is 190～300 ℃, and the air outlet temperature is 90～150 ℃.
The molybdenum powder that MP-1 requires in the general accord with Q of above-mentioned raw materials molybdenum powder/JDC013-2002 standard, Fisher particle size is 1.5～4 μ m, apparent density is 0.8～1.5g/cm3, impurity content＜0.5%.
Above-mentioned Metal Ball can be any of molybdenum ball, stainless steel ball, sintered carbide ball, and shape is not limited to sphere.
Above-mentioned polyethylene glycol is a number-average molecular weight from any of 600～3000 polyethylene glycol.
Above-mentioned Metallic stearates can be any of stearic acid, zinc stearate, odium stearate, dolomol, calcium stearate.
Above-mentioned polyacrylic acid ammonium salt solution is colourless or light yellow transparent liquid, and the mass fraction of solute is 10%～50%.
The atomizing type of above-mentioned spray drying tower can be centrifugal atomizing formula and spray gun pressure formula.
Because the present invention has carried out certain optimization to the prescription of binder solution, and be that the raw material molybdenum powder fully mixes with binder solution, formed even molybdenum powder slip through effective wet-milling mode.Making the molybdenum powder of preparation can directly be used for automatic extruding through spraying granulation technology is shaped.This method has following advantage:
(1) can a step prepare the molybdenum powder that is suitable for automatic forming, need not carry out follow-up loaded down with trivial details processing, production efficiency is high, and cost is low.
(2) powder flowbility for preparing of the present invention is good, and apparent density is high, and size distribution is suitable, and has the effect of self-lubricating, can directly be used for automatic extruding and be shaped.
(3) because the solvent that uses among the present invention is water, can there be environmental pollution problems in industrialization.
The automatic forming of (4) producing is difficult for the moisture absorption with molybdenum powder, and moisture content is suitable for automatic extruding production less than 0.2% very much.
(5) carbon, oxygen content are all less than 100ppm behind the molded product sintering, and sintered density is higher than 97%.
Description of drawings
Fig. 1 is the process chart of the inventive method.
Fig. 2 is the automatic forming for preparing through the embodiment 4 surface sweeping electromicroscopic photograph with molybdenum powder: a is 100 times of overall photos; B is 1000 times of individual particle photos; C is 4000 times of fine structure photos.
The specific embodiment
Through embodiment the present invention is specifically described below; Be necessary to be pointed out that at this following examples only are used for the present invention is further specified; Can not be interpreted as the restriction to protection domain of the present invention, the person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to above-mentioned fermentation content.
What be worth explanation is to form added umber in following examples and be mass parts.
Embodiment 1
200 parts of pure water, 5 parts of polyvinyl alcohol, 1 part of polyethylene glycol are stirred down at 80～90 ℃ and be modulated into binder solution in 2 hours.To ask for 1000 parts of raw material molybdenum powders according to MP-1 in the Q/JDC013-2002 standard, with these 1000 parts of raw material molybdenum powders, 3000 parts of sintered carbide balls, put into the wet-milling of roller ball grinding machine with 206 parts of 20.6% the binder solution of being modulated that is equivalent to raw material molybdenum powder weight and mix and be prepared into the molybdenum powder slip in 18 hours.Open air-introduced machine, pressure fan and the heating system of spray drying tower in order, use pure water to spray in advance.The intake air temperature that spray drying tower is set is 260 ℃, and the air outlet temperature is 130 ℃, and is subsequent use after regulating.The molybdenum powder slip is squeezed into spray drying tower inside through membrane pump and spray gun carry out drying and granulating.Discharging opening at spray drying tower is collected through vibratory sieve.
Embodiment 2
300 parts of pure water, 13 parts of polyvinyl alcohol, 2 parts of polyethylene glycol are stirred down at 80～90 ℃ and were modulated into binder solution in 2 hours.To ask for 1000 parts of raw material molybdenum powders according to MP-1 in the Q/JDC013-2002 standard, with these 1000 parts of raw material molybdenum powders, 3000 parts of stainless steel balls, put into the wet-milling of roller ball grinding machine with 315 parts of 31.5% the binder solution of being modulated that is equivalent to raw material molybdenum powder weight and mix and be prepared into the molybdenum powder slip in 36 hours.Open air-introduced machine, pressure fan and the heating system of spray drying tower in order, use pure water to spray in advance.The intake air temperature that spray drying tower is set is 265 ℃, and the air outlet temperature is 130 ℃, and is subsequent use after regulating.The molybdenum powder slip is squeezed into spray drying tower inside through membrane pump and spray gun carry out drying and granulating.Discharging opening at spray drying tower is collected through vibratory sieve.
Embodiment 3
500 parts of pure water, 25 parts of polyvinyl alcohol, 4 parts of polyethylene glycol are stirred down at 80～90 ℃ and were modulated into binder solution in 2 hours.To ask for 1000 parts of raw material molybdenum powders according to MP-1 in the Q/JDC013-2002 standard, with these 1000 parts of raw material molybdenum powders, 2000 parts of molybdenum balls, put into the wet-milling of roller ball grinding machine with 529 parts of 52.9% the binder solution of being modulated that is equivalent to raw material molybdenum powder weight and mix and be prepared into the molybdenum powder slip in 10 hours.Open air-introduced machine, pressure fan and the heating system of spray drying tower in order, use pure water to spray in advance.The intake air temperature that spray drying tower is set is 200 ℃, and the air outlet temperature is 100 ℃, and is subsequent use after regulating.The molybdenum powder slip is squeezed into the centrifugal atomizing dish of spray-drying top of tower through membrane pump and carrier pipe, through the high speed rotary-atomizing molybdenum powder slip and the drying and granulating of centrifugal atomizing dish.Discharging opening at spray drying tower is collected through vibratory sieve.
Embodiment 4
350 parts of pure water, 14 parts of polyvinyl alcohol, 2 parts of polyethylene glycol are stirred down at 80～90 ℃ and were modulated into binder solution in 2 hours.To ask for 1000 parts of raw material molybdenum powders according to MP-1 in the Q/JDC013-2002 standard, with these 1000 parts of raw material molybdenum powders, 3000 parts of molybdenum balls, put into the wet-milling of roller ball grinding machine with 366 parts of 36.6% the binder solution of being modulated that is equivalent to raw material molybdenum powder weight and mix and be prepared into the molybdenum powder slip in 18 hours.Open air-introduced machine, pressure fan and the heating system of spray drying tower in order, use pure water to spray in advance.The intake air temperature that spray drying tower is set is 220 ℃, and the air outlet temperature is 115 ℃, and is subsequent use after regulating.The molybdenum powder slip is squeezed into the centrifugal atomizing dish of spray-drying top of tower through membrane pump and carrier pipe, through the high speed rotary-atomizing molybdenum powder slip and the drying and granulating of centrifugal atomizing dish.Discharging opening at spray drying tower is collected through vibratory sieve.
Embodiment 5
It is subsequent use at first weight to be that 3 parts stearic acid is dissolved in 10 parts of ethanol the stearic ethanolic solution of preparation.Then 340 parts of pure water, 14 parts of polyvinyl alcohol, 2 parts of polyethylene glycol are stirred fully dissolving in 2 hours down at 80～90 ℃, the cooling back adds the stearic ethanolic solution of preparation, and 2 parts of polyacrylic acid ammonium salt solutions fully stir and were modulated into binder solution in 1 hour.To ask for 1000 parts of raw material molybdenum powders according to MP-1 in the Q/JDC013-2002 standard, with these 1000 parts of raw material molybdenum powders, 3000 parts of molybdenum balls, put into the wet-milling of roller ball grinding machine with 371 parts of 37.1% the binder solution of being modulated that is equivalent to raw material molybdenum powder weight and mix and be prepared into the molybdenum powder slip in 18 hours.Open air-introduced machine, pressure fan and the heating system of spray drying tower in order, use pure water to spray in advance.The intake air temperature that spray drying tower is set is 230 ℃, and the air outlet temperature is 120 ℃, and is subsequent use after regulating.The molybdenum powder slip is squeezed into the centrifugal atomizing dish of spray-drying top of tower through membrane pump and carrier pipe, through the high speed rotary-atomizing molybdenum powder slip and the drying and granulating of centrifugal atomizing dish.Discharging opening at spray drying tower is collected through vibratory sieve.
Embodiment 6
It is subsequent use at first weight to be that 3 parts stearic acid is dissolved in 10 parts of ethanol the stearic ethanolic solution of preparation.Then 400 parts of pure water, 13 parts of polyvinyl alcohol, 2 parts of polyethylene glycol are stirred fully dissolving in 2 hours under 80～90 ℃, the stearic ethanolic solution that adds preparation after the cooling fully stirs and was modulated into binder solution in 1 hour.To ask for 1000 parts of raw material molybdenum powders according to MP-1 in the Q/JDC013-2002 standard, with these 1000 parts of raw material molybdenum powders, 1000 parts of molybdenum balls, put into the wet-milling of roller ball grinding machine with 428 parts of 42.8% the binder solution of being modulated that is equivalent to raw material molybdenum powder weight and mix and be prepared into the molybdenum powder slip in 18 hours.Open air-introduced machine, pressure fan and the heating system of spray drying tower in order, use pure water to spray in advance.The intake air temperature that spray drying tower is set is 240 ℃, and the air outlet temperature is 130 ℃, and is subsequent use after regulating.The molybdenum powder slip is squeezed into the centrifugal atomizing dish of spray-drying top of tower through membrane pump and carrier pipe, through the high speed rotary-atomizing molybdenum powder slip and the drying and granulating of centrifugal atomizing dish.Discharging opening at spray drying tower is collected through vibratory sieve.
Embodiment 7
With 350 parts of pure water, 20 parts of polyvinyl alcohol, 3 parts of polyethylene glycol fully dissolvings after stirring 2 hours under 80～90 ℃, adding 2 parts of polyacrylic acid ammonium salt solutions in cooling back fully stir and were modulated into binder solution in 1 hour.To ask for 1000 parts of raw material molybdenum powders according to MP-1 in the Q/JDC013-2002 standard, with these 1000 parts of raw material molybdenum powders, 3000 parts of molybdenum balls, put into the wet-milling of roller ball grinding machine with 375 parts of 37.5% the binder solution of being modulated that is equivalent to raw material molybdenum powder weight and mix and be prepared into the molybdenum powder slip in 18 hours.Open air-introduced machine, pressure fan and the heating system of spray drying tower in order, use pure water to spray in advance.The intake air temperature that spray drying tower is set is 220 ℃, and the air outlet temperature is 115 ℃, and is subsequent use after regulating.The molybdenum powder slip is squeezed into the centrifugal atomizing dish of spray-drying top of tower through membrane pump and carrier pipe, through the high speed rotary-atomizing molybdenum powder slip and the drying and granulating of centrifugal atomizing dish.Discharging opening at spray drying tower is collected through vibratory sieve.
For the better premium properties of the molybdenum powder of explanation the present invention preparation, table 1 has been listed key property, size distribution situation and the moisture content of the prepared automatic forming of the foregoing description with molybdenum powder.
The prepared automatic forming of table 1 the foregoing description is tabulated with the performance of molybdenum powder
Claims (5)
1. an automatic forming is used special molybdenum powder; It is characterized in that consisting of of this special molybdenum powder: the mass fraction of raw material molybdenum powder is 96.6～99.5; The mass fraction of polyvinyl alcohol is 0.5～2.4; The mass fraction of polyethylene glycol is 0～0.4, and the mass fraction of Metallic stearates is for being 0～0.5, and the mass fraction of ammonium polyacrylate is 0～0.15.
2. method for preparing the described automatic forming of claim 1 with special molybdenum powder, the processing step of this method is following:
(1) binder of preparation polyvinyl alcohol, polyethylene glycol, water, Metallic stearates and ammonium polyacrylate
Solution;
(2) raw material molybdenum powder, Metal Ball and above-mentioned binder solution are carried out wet-milling in proportion in ball grinder and be mixed with the molybdenum powder slip;
(3) the molybdenum powder slip with preparation carries out spray-drying process;
(4) molybdenum powder that makes is collected through spray drying tower discharging opening vibratory sieve.
3. the method for preparing automatic forming with special molybdenum powder according to claim 2, the process for preparation that it is characterized in that described binder solution are that at first weight to be that 0～5 part of Metallic stearates is dissolved in 10 parts of ethanol the ethanolic solution of preparation Metallic stearates subsequent use; Be 200～500 parts pure water then with weight; 5～25 parts polyvinyl alcohol; 0～4 part polyethylene glycol stirs fully dissolving in 2 hours under 80～90 ℃ temperature; The cooling back adds the ethanolic solution of the Metallic stearates of preparation, and 0～2 part polyacrylic acid ammonium salt solution fully stirs and was modulated into binder solution in 1 hour.
4. the method for preparing automatic forming with special molybdenum powder according to claim 2; The preparation process that it is characterized in that the molybdenum powder slip is with the raw material molybdenum powder, for the Metal Ball of raw material molybdenum powder weight 100%～300%, puts into the roller ball grinding machine for the above-mentioned binder solution of raw material molybdenum powder weight 20.5～54.6% and carry out wet-milling and mix, and the wet-milling time is 10～36 hours.
5. the method for preparing automatic forming with special molybdenum powder according to claim 2, what it is characterized in that its spray-drying process process employing is spray drying tower, and the intake air temperature of spray drying tower is 190～300 ℃, and the air outlet temperature is 90～150 ℃.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102615288A (en) * | 2012-03-26 | 2012-08-01 | 宁波福沃德新材料科技有限公司 | Method for preparing spherical metal molybdenum particles for cold spraying |
| CN102626784B (en) * | 2012-05-10 | 2014-01-01 | 金堆城钼业股份有限公司 | Method for preparing molybdenum powder for preparing molybdenum end cap of magnetron |
| CN103028859A (en) * | 2012-06-08 | 2013-04-10 | 厦门虹鹭钨钼工业有限公司 | Solder ring for magnetron cathode assembly, method for producing solder ring for magnetron cathode assembly and molybdenum end cap connecting with solder ring |
| CN103170635B (en) * | 2013-03-29 | 2015-10-21 | 金堆城钼业股份有限公司 | A kind of method preparing spherical molybdenum powder |
| CN104230314A (en) * | 2013-06-14 | 2014-12-24 | 上海好景新型陶瓷材料有限公司 | Environmental-friendly full-automatic production device for aluminum oxide ceramic pelleting powder |
| CN105397094B (en) * | 2015-12-23 | 2018-06-15 | 北京矿冶研究总院 | Preparation method of spherical spraying molybdenum powder |
| CN105642881A (en) * | 2016-03-16 | 2016-06-08 | 江西耀升钨业股份有限公司 | Technology for producing hard alloy woodworking blade by means of fine-particle return scraps |
| CN106424702B (en) * | 2016-09-12 | 2018-06-29 | 黑龙江北方工具有限公司 | A kind of tungsten alloy binder and its preparation method and application |
| CN108115147A (en) * | 2017-12-04 | 2018-06-05 | 中国兵器科学研究院宁波分院 | A kind of complete closely knit, the spherical molybdenum powder of high apparent density the preparation method of cold spraying |
| CN109175353B (en) * | 2018-09-13 | 2021-05-11 | 北京有研粉末新材料研究院有限公司 | Surface coating method for automatic pressing and forming of spherical powder |
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