CN1340392A - Prilling of metal powder or ceramic powder and its making method and manufacture method of sintered material with prilling powder as raw material - Google Patents
Prilling of metal powder or ceramic powder and its making method and manufacture method of sintered material with prilling powder as raw material Download PDFInfo
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- CN1340392A CN1340392A CN 01121760 CN01121760A CN1340392A CN 1340392 A CN1340392 A CN 1340392A CN 01121760 CN01121760 CN 01121760 CN 01121760 A CN01121760 A CN 01121760A CN 1340392 A CN1340392 A CN 1340392A
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Abstract
In a sintered material used in the process of granulating the fine powder of metal powder, there has been a danger of causing ignition or vaporization, further, there has been no binders having low concentration and exhibiting high viscosity, whereby the formation of a homogeneous slurried viscous liquid with metal powder having remarkably different specific gravity has been impossible, moreover, there has been a need of performing a degreasing stage in the existent binders, additionally, there has been a need of using die steel withstanding high pressure in the conventional powder metallurgy method, and further, the formation of a product having a complicated shape has been impossible. As a binder, natural high-molecular polysaccharides having sol viscosity of 2% concentration and exhibiting viscosity of >=300 mPa.s are used. As the natural high-molecular polysaccharides, particularly, high viscosity agar is desirable. The granulated body using the above binder has the characteristics of being extremely high in rigidity and further has the characteristics of being enough in workability.
Description
The present invention relates to usually metal dust, ceramic powders compression are formed into body, this formed body is carried out sintering, make the powder metallurgic method of sintered article with rigidity.In more detail, the new prilling process of the material powder before the present invention relates to be shaped will be by the method for the prilling powder compression molding of this prilling process preparation, and obtains the more complicated sintered products of shape by this formed body being carried out machining.
With the metal dust granulation and form metal granulation powder, the basic fundamental that adopts the compressed shaping/degreasing of this granulation powder/all operations of sintering to form the powder metallurgic method of required goods is long ago to develop and widely used in industrial circle.On the other hand, by the machining metal to found the machining method that material cuts out with given shape be more widely used always before this.
In the machining method of cutting out with given shape, can produce a large amount of cutting swarfs by the saw lumber of machining Metal Melting.Usually, these cutting swarfs are according to the lifting of old metal price, the principle of economic aspect, handle by the methods such as landfill that are not described.But, recently, angle from environmental protection, particularly as a method of the problem that solves the disposal of industrial wastes etc., compare with the machining method that produces a large amount of cutting swarfs, a large amount of sintered components of producing by the powder metallurgic method with few this advantage of cutting swarf generation that use are by conscientious research.
So far, adopt powder metallurgic method, as bond material the fine powder of metal dust is carried out granulation with organic polymer and organic solvent, improve the flowability of metal dust, by using the metal granulation powder that makes like this, but automatic gauge and automatic forming so just can obtain the body that is compressed into of homogeneous more.Then, by this formed body being carried out ungrease treatment and in sintering furnace, carrying out sintering, obtain sintered body.When making the sintered body of the complicated shape that can't obtain by the single shaft shaping, the presintering operation was set before this sintering, the presintering body that machining obtains by presintering then, by this machining body of this sintering, is made the sintered body of complicated shape.
The particle diameter of employed material powder is to the such wide region of tens of microns from several microns in the powder metallurgic method, be under several microns the situation of micro mist at particle diameter, particularly the flowability of powder is poor, the density unevenness of formed body, it is inhomogeneous to cause sintering to shrink thus, and the dimensional accuracy of sintered body is than given value difference.In order to address this problem,, use the powder of this granulation to carry out thermal sintering in advance with the metal dust granulation.Carry out in the process of granulation at micro mist,, water-fast organic high molecular compound such as wax, acrylic resin, camphor is dissolved in the organic solvents such as carrene and uses as binding material to metal dust.If exist from the residual carbon of organic high molecular compound is superfluous, the overslaugh in the time of can causing sintering is shunk, and reduces the mechanical property value of sintered body.In order to address this problem, the degreasing process of removal as the water-fast organic high molecular compounds such as wax, acrylic resin and camphor of binding material use must be arranged, and then special equipment and the technology of these operation needs, discharge harmful decomposition gas, perhaps cause the generation of stench.And organic solvent has the danger of catching fire, gasify easily and discharge into the atmosphere, cause easily the problem of atmosphere pollution.
One of feature of powder metallurgic method is by mixing multiple metal material with arbitrary proportion, can preparing the alloy with special nature at an easy rate.But must form the necessary material of alloy for this reason, i.e. the great metal dust of specific gravity difference, for example tungsten and copper, molybdenum and copper, even and then mixed-powders such as tungsten and aluminium, also must the homogeneous granulation.For example, carry out the homogeneous granulation, must inhale with pump and carry the pulp-like viscous liquid that mixture and binding material by the very large metal dust of specific gravity difference form, it is supplied to the sprayer unit that rotates at a high speed in order to adopt spray drying process.Because the mixture of this metal dust and binding material constitute homogeneous pulp-like viscous liquid, have the such problem of full-bodied binding material under the low concentration so exist must be chosen to be at.
Adopt spray drying process, in the mixture of metal dust, mix and have that fillibility and the mould that prevents to adhere are the wax and the fatty acid of purpose when being shaped as the organic high molecular compound of binding material function with to improve, carry out granulation, but when using these binding materials, existing in sintering before must be through the problem of degreasing process.
In iron-based alloy with the powder of easy plastic deformation during as raw material, in order to improve sintered density, need be at the high pressure of feed metal powder generation plastic deformation degree, for example the high pressure of 500～700MPa is shaped down.Must select the such problem of die steel of ability high pressure like this when therefore existing in mfg. moulding die.
Shaping operation is from the pressurization of single shaft direction basically and is shaped.But, recently, to carry out with the effort that obtains the more complicated formed products of shape in order to adopt mould with the complicated structure that is assembled into slide construction always, this effort also has the limit.In order to obtain more complicated shape, can consider machining shaping product.But what existence caused owing to formed products intensity is low can't bear the problem that cutting element rotates the destructive power of being brought, or the frictional heat of cutting element causes the problem that formed body expands and breaks.
Except being the situation of raw material with the tungsten based metal powder, in order to prepare the goods of the complicated shape that can't obtain, can before this sintering, under than the also low low temperature of common sintering temperature, prepare the presintering body by compression molding, this presintering body is carried out machining.But the cutting swarf that is accompanied by this machining generation is not suitable for recycling profit again, so there is the problem that must carry out landfill disposal.
In order to solve above-mentioned problems, in the present invention, binding material uses that to have dissolved adhesiveness be 2% o'clock natural macromolecule amylose class as the viscosity more than the 300mPa.s in concentration, wishes it is a kind of high viscosity agar in the natural macromolecule amylose class especially.
The preferred embodiments of the present invention are below described.But the present invention should not be understood that to only limit to these embodiments.The compression molding of proportion for extremely different raw meal described among the embodiment 1.The compression molding of high specific gravity tungsten carbide system has been described among the embodiment 2.Description is the compression molding of raw material with the meal of the steel SUS316L of easy plastic deformation among the embodiment 3.
Embodiment 1
The adding average grain diameter is 2.0 microns carbonyl nickel and a carbonyl iron powder in the tungsten powder of 2.0 microns of average grain diameters, their amount is respectively 3 weight %, 1.5 weight %, the wet mixed that adopts automatic mixer to carry out two hours is carried out drying, makes material powder.Then, in this material powder of 9.05kg, add dissolved adhesiveness concentration be 2% o'clock be the high viscosity agar solution 1.72kg of 900mPa.s, under near the temperature 60 ℃, be incubated, stir simultaneously, make mud shape liquid.The spray drier that this mud shape liquid employing condition is 25000rpm, 160 ℃ of inlet temperatures, 78 ℃ of outlet temperatures is sprayed, make 30～50 microns spherical prilling powder.Use the withstand voltage intensity that contracts of the formed body of this prilling powder to represent at table-1.And,, also list the withstand voltage intensity that contracts of the formed body of under the forming pressure of 100MPa and 300MPa, making as binding material with employed acrylic resin and carrene in the present conventional powder metallurgic method in order to compare.Table 1
The withstand voltage intensity that contracts (unit) MPa of formed body
| Binding material | Forming pressure | The withstand voltage intensity that contracts |
| Binding material of the present invention | ????50 | ?????3.24 |
| ?????????″ | ????70 | ?????4.35 |
| ?????????″ | ????100 | ?????5.48 |
| Existing binding material | ????100 | ?????1.23 |
| ?????????″ | ????300 | ?????4.20 |
By this table 1 as seen, binding material of the present invention has than withstand voltage the contract intensity higher value of existing binding material at 300MPa in the withstand voltage intensity that contracts of 70MPa.
This prilling powder is put into the mould of given shape, under the pressure of 300MPa, carry out press molding and obtain formed body, then, this formed body decomposed in 400 ℃ steam atmosphere remove agar, measure the residual carbon amount that this removes gas, the result is 0.001 weight %, have with initiation material in the same degree of tungsten.
Then, this is removed gas in steam, in 1460 ℃ the stove, carry out sintering, carry out the liquid-phase sintering of Ni-Fe binder course fusion, obtain tungsten particle and directly be 50 microns sintered body.The dimensional accuracy that obtains sintered article is ± the following high sintered article of precision of 0.01mm that the hardness of sintered article is expressed as 330 with Vickers hardness, has the plastic deformation ability of very anti-riveted joint processing, is durable goods.
Embodiment 2
The cobalt dust that the tungsten-carbide powder that the average grain diameter of weighing 82% is 2.5 microns, 8% titanium carbide powder and 10% average grain diameter are 2.0 microns, adopt automatic mixer to carry out 50 hours wet mixed after, drying is made material powder.Then, adding dissolved adhesiveness in 7.5 kilograms of these material powders is 2% o'clock to be 1.72 kilograms of the high viscosity agar solutions of 900mPa.s in concentration, keeps temperature under the temperature about 60 ℃, stirs simultaneously, makes mud shape liquid.It is that 25000rpm, inlet temperature are that 160 ℃, outlet temperature are in 78 ℃ the spray drier that this mud shape liquid is sprayed to condition, makes 20～30 microns spherical prilling powder.
This prilling powder is added in the mould of given shape, press molding under the pressure of 100MPa obtains formed body, then, this formed body by in 400 ℃ the stove that contains steam, is decomposed and to remove agar, carries out sintering under 1450 ℃ in a vacuum.Then, the HIP that carried out 1 hour in 1350 ℃, the argon gas of 100MPa handles, and obtains sinter.Measure the fracture resistence force of this sinter, the result is 3～3.7GPa, and is suitable with general superhard alloy.
Embodiment 3
Adding dissolved adhesiveness in the water atomization powder of the SUS316L of 66 microns of 1 kilogram of average grain diameters is 2% o'clock to be 0.4 kilogram of the high viscosity agar solution of 900mPa.s in concentration, after fully stirring and carrying out cooling curing, in that this cured block is pulverized, under 60～80 ℃, carry out drying then.And then, pulverize repeatedly and sieve, make particle diameter at the granulation powder below 297 microns.With stainless steel granulation powder press molding under 200MPa, 400MPa and 600Mpa of this SUS316L, measure the compressive strength of formed body, the result represents at table 2.In order to compare, also represented in the existing conventional powder metallurgic method employed with polyvinyl alcohol and stearic acid the withstand voltage intensity that contracts as bond material and the formed body under the forming pressure of 600MPa, made.Table 2
Withstand voltage intensity (the unit: MPa) that contracts of formed body
| Bond material | Forming pressure | The withstand voltage intensity that contracts |
| Bond material of the present invention | ????200 | ?????63.08 |
| ???????″ | ????400 | ?????138.26 |
| ???????″ | ????600 | ?????238.55 |
| Existing bond material | ????600 | ?????26.55 |
By this table 2 as seen, bond material of the present invention is compared in the withstand voltage intensity that contracts of 600MPa with existing bond material in the withstand voltage intensity that contracts of 200～600MPa, and has the value that is higher than it far away.In addition, the formed products that the granulation powder that adopts the inventive method to prepare is made in the shaping of 400MPa lower compression adopts end mill to carry out high speed and cuts, and its state is shown in the photo in the accompanying drawing 1.
The photo of accompanying drawing 1 is represented the machining state of press molding body
As shown in Figure 1, the visible following fact is even namely also can't see defective on the edge.
This prilling powder that in the mould that is shaped as projection size 20 * 60mm, adds 90g, under the pressure of 400MPa, carry out press molding, after obtaining formed body, adopting diameter is the twolip vice steel end mill of 8mm, be that 4 millimeters, end mill revolution are to carry out full cutter processing under the processing conditions of 2000rpm, single-blade feed 0.05mm in penetraction depth, in a vacuum 1350 ℃ of lower maintenances 2 hours, obtain sinter. Obtain sintering shrinkage power 9.65%, density 6.85g/mm3Sinter, suitable with the sinter that is obtained by existing powder metallurgic method.
The invention effect
Carry out in the operation of granulation at micro mist metal dust, the degreasing process of removing the water-fast organic high molecular compounds such as wax, acrylic resin and camphor that use as bond material must be arranged, also exist in addition and need special equipment and technology in this operation, discharge the problem that harmful decomposition gas causes stench, and then the danger that exists organic solvent to catch fire, gasification discharges the problems that cause atmosphere pollution in atmosphere easily, and these problems are all solved as bond material by using the natural macromolecule amylose class.The natural macromolecule amylose class particularly agar only with water as solvent, the danger of not only not catching fire, and do not worry the atmosphere pollution that in atmosphere, volatilizees fully.
To have dissolved adhesiveness be that 2% o'clock class as the natural macromolecule amylose class of the viscosity of 300MPa is that high viscosity agar is as bond material in concentration by using, to be oar shape viscous liquid have high viscosity more than the 500mPa.s 70 ℃ viscosity to the mixture of great metal dust of specific gravity difference and 2% agar solution, and then by by mixer with the above revolution of 100rpm, the metal dust that above-mentioned specific gravity difference is big is present in and carries out granulation in the spray-drying, has solved the problem of the different granulation powder of preparation bond material ratio fully.
In spray drying process, the bond material that uses organic high molecular compound, wax and fatty acid to be mixed and made into carries out granulation, at this moment, degreasing process that must be before oversintering, as described herein, by using agar as bond material, can save degreasing process fully, this is known (special fair 7-68566 number) the inventor
In iron-based alloy, during as raw material,, must select high voltage bearing golden structural section,, just not need such selection by using the natural macromolecule amylose class as bond material in order to improve sintered density with the powder of easy generation plastic deformation.This is that withstand voltage the contract intensity of bond material of the present invention under 70MPa is compared with the withstand voltage intensity that contracts of existing bond material under 300Mpa, has higher value because by above-mentioned table 1 as seen.
In addition, use the natural macromolecule amylose class as bond material, in being 66 microns the water atomization powder of SUS316L, 1 kilogram of average grain diameter adds that to have dissolved adhesiveness be to be 0.4 kilogram of the high viscosity agar solution of the viscosity of 900mPa.s in concentration at 2% o'clock, fully stir, after the cooling curing, pulverize this cured block, under 60～80 ℃, carry out drying then, pulverize repeatedly and sieve, make particle diameter at the granulation powder below 297 microns, by with the stainless steel granulation powder of this SUS316L at 200MPa, carry out press molding under 400MPa and the 600MPa and make formed body, shown in above-mentioned table 2, can make the withstand voltage formed body of intensity that contract far above the formed body that uses existing bond material.Therefore, according to the present invention, in order to obtain more complicated shape, even when machining has the formed body of the high withstand voltage intensity that contracts, the also machining body that can not expanded and isolate.
In addition, as shown in the present, with the natural macromolecule amylose class particularly agar obtain formed body as SUS316L stainless steel granulation powder press molding under 400MPa of bond material, adopt end mill to carry out high-speed cutting this formed body, at this moment the cutting swarf of Chan Shenging is different fully with the form of original raw material powder under the such weak sintering condition of false sintering, therefore, can reuse by direct recovery or the granulation powder of making compression molding, perhaps, turn back in the granulating working procedure to mix and re-use with new raw meal.Therefore, can solve the problem of environmental pollution that the cutting swarf landfill disposal is brought really as mentioned above.
Claims (7)
1. prilling powder, this powder are the prilling powders of being made by metal dust that uses as agglomerated material or ceramic powders, it is characterized in that carrying out granulation with the natural macromolecule amylose class as bond material.
2. the manufacturing process of a prilling powder, this method are the prilling powder manufacturing process of the prilling powder of shaping claim 1 record, it is characterized in that using as bond material with the natural macromolecule amylose class.
3. prilling powder manufacturing process as claimed in claim 2 is characterized in that said natural macromolecule amylose class is an agar.
4. as claim 2 or 3 described prilling powder manufacturing process, it is characterized in that adopting spray drying process to carry out granulation.
5. prilling powder manufacturing process as claimed in claim 3 is characterized in that adding aqueous agar solution in metal dust or ceramic powders, it is stirred to mix, and carries out drying and pulverizing then, carries out granulation thus.
6. the prilling powder that manufacture method of making agglomerated material, this method will adopt the method for any record of claim 2～5 to be shaped and make is made agglomerated material by compress moulding method and/or sintering method.
7. manufacture method of making final agglomerated material, this method is carried out machining to the formed body that the manufacture method by claim 6 record is shaped, only be processed into the shape that can't obtain by compression molding after, carry out sintering again.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000255702A JP2002069505A (en) | 2000-08-25 | 2000-08-25 | Granulation of metal powder or ceramic powder, its production method and method for producing sintered material using the granulated powder as raw material |
| JP255702/2000 | 2000-08-25 |
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| Publication Number | Publication Date |
|---|---|
| CN1340392A true CN1340392A (en) | 2002-03-20 |
| CN1272126C CN1272126C (en) | 2006-08-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 01121760 Expired - Fee Related CN1272126C (en) | 2000-08-25 | 2001-07-06 | Prilling of metal powder or ceramic powder and its making method and manufacture method of sintered material with prilling powder as raw material |
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| JP (1) | JP2002069505A (en) |
| CN (1) | CN1272126C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107583111A (en) * | 2017-10-31 | 2018-01-16 | 张蕴萍 | A kind of micro- profitization processing method of catheter surface |
| CN109534828A (en) * | 2019-01-10 | 2019-03-29 | 广东昭信照明科技有限公司 | A kind of prilling process of silicon carbide composite ceramic materials |
| CN111116211A (en) * | 2019-12-27 | 2020-05-08 | 中铭瓷(苏州)纳米粉体技术有限公司 | Preparation method of ternary nano lamellar MAX phase powder and product thereof |
-
2000
- 2000-08-25 JP JP2000255702A patent/JP2002069505A/en active Pending
-
2001
- 2001-07-06 CN CN 01121760 patent/CN1272126C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107583111A (en) * | 2017-10-31 | 2018-01-16 | 张蕴萍 | A kind of micro- profitization processing method of catheter surface |
| CN109534828A (en) * | 2019-01-10 | 2019-03-29 | 广东昭信照明科技有限公司 | A kind of prilling process of silicon carbide composite ceramic materials |
| CN111116211A (en) * | 2019-12-27 | 2020-05-08 | 中铭瓷(苏州)纳米粉体技术有限公司 | Preparation method of ternary nano lamellar MAX phase powder and product thereof |
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| Publication number | Publication date |
|---|---|
| JP2002069505A (en) | 2002-03-08 |
| CN1272126C (en) | 2006-08-30 |
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