CN102806355A - Powder metallurgy fabrication method of hollow metal sphere - Google Patents

Powder metallurgy fabrication method of hollow metal sphere Download PDF

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CN102806355A
CN102806355A CN 201210315834 CN201210315834A CN102806355A CN 102806355 A CN102806355 A CN 102806355A CN 201210315834 CN201210315834 CN 201210315834 CN 201210315834 A CN201210315834 A CN 201210315834A CN 102806355 A CN102806355 A CN 102806355A
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step
metal powder
suspension
mold
slurry
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CN 201210315834
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Chinese (zh)
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迟煜頔
王建
谈萍
王辉
荆鹏
陈金妹
康新婷
杨坤
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西北有色金属研究院
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Abstract

The invention discloses a powder metallurgy fabrication method of a hollow metal sphere, which comprises the following steps of placing a polystyrene sphere in a centrifugal mold, preparing slurry 1 with metal powder, adhesive solution and a defoaming agent, pouring the slurry 1 into the centrifugal mold, centrifuging, putting the centrifuged polystyrene sphere in an oven for drying together with the centrifugal mold, preparing slurry 2 with the metal powder, the adhesive solution and the defoaming agent, pouring the slurry 2 into the dried centrifugal mold, centrifuging, putting the centrifuged polystyrene sphere in the oven for drying together with the centrifugal mold, taking out the dried polystyrene sphere from the centrifugal mold, embedding the polystyrene sphere into alumina packing, and then putting in a vacuum furnace for pyrolysis and sintering, thereby obtaining the hollow metal sphere. The method is reasonable in design, simple in process and low in cost. The hollow metal sphere fabricated by the fabrication method has the advantages of uniform, smooth and complete spherical shell wall thickness, facilitation of sphere dimension selection, easiness in overall structure control and the like.

Description

一种金属空心球的粉末冶金制备方法 Powder metallurgy method for producing a metallic hollow balls

技术领域 FIELD

[0001] 本发明属于金属空心球制备技术领域,尤其是涉及一种金属空心球的粉末冶金制备方法。 [0001] The present invention belongs to the technical field of producing metal hollow spheres, particularly to a hollow metal sphere with powder metallurgy method.

背景技术 Background technique

[0002]目前的热防护体系中间部分所采用的隔热材料一般为氧化铝陶瓷纤维,虽然它质轻,耐热性强以及抗氧化性好,但抗热震性差,导热率随温度的变化很大,而且由于非金属和金属盖板间热膨胀系数的差异,容易引起热循环中的结构不稳定性。 [0002] Current thermal insulating material intermediate portion protection system is generally used alumina ceramic fiber, though it is light weight, high heat resistance and good oxidation resistance, thermal shock resistance but poor thermal conductivity variation with temperature large, but due to the difference in thermal expansion coefficient between the metal and non-metal plate, structural instability prone to thermal cycling. 而由烧结或连接空心球颗粒制备的空心球金属泡沫内部空心,球壳致密是一种兼具功能和结构双重属性的新型功能材料,能有效地抑制对流和辐射传热。 Sintered particles prepared by a hollow sphere or hollow sphere connecting metal foam inside the hollow spherical shell dense material is a function of both function and structure are novel dual nature, can effectively suppress convection and radiation heat transfer. 在发动机、燃烧室等高温环境下的缓冲防护、降噪隔热等方面有潜在应用。 It has potential applications in terms of cushioning, insulation, and other noise in the engine, a combustion chamber high temperature environment.

[0003]目前金属空心球的制备方法有雾化法、金属流化床法和滚粉烧结法等。 [0003] The present method for preparing metal hollow spheres with a spray method, a metal rolling method and fluidized-bed powder sintering method and the like. 雾化法产量低(通常只有1%〜5%),而且获得的空心球的尺寸较小;金属流化床法从理论上讲可以制备任何金属及合金的空心球材料,但工序复杂,成本较高;滚粉烧结法制备的空心球表面干燥,壁薄且不易控制,球与球之间需要采用合金粉浆加以粘接,制备效率很低。 Yield Low atomizing method (typically only 1% ~ 5%), and the smaller the size of the obtained hollow spheres; fluidized bed process may be prepared by any metal hollow sphere material of metals and alloys in theory, but the process is complicated, the cost high; prepared by powder sintering method roller hollow spherical surface drying, thin-walled and difficult to control, we need slip between the balls and the alloy to be adhered, low production efficiency. 目前国际、国内对金属空心球材料制备工艺控制的理论研究极为薄弱。 At present theoretical study of international, domestic metal manufacturing process control materials is also very weak. 以上几种方法都存在球体尺寸不易控制、球壳表面完整性差、球壳壁厚不均匀等现象。 Several methods are difficult to control the size of the sphere is present, spherical shell surface integrity is poor, uneven wall thickness of the spherical shell phenomena.

[0004] 离心沉积制备的优点很多,主要包括操作步骤简便且生产成本低廉,可应用材料广泛、成型速度快等优点。 Many advantages [0004] Preparation of centrifugal deposition, including the steps simple and inexpensive to produce, can be widely applied material, the advantages of rapid speed molding. 但在现有研究技术中,金属空心球制备技术的相关报导很多,但用此法制备金属空心球结构材料的工艺及理论研究,国内外暂无报导,也没有相关专利。 However, in the prior art research, a metal hollow spheres preparation technology many stories, but the process and theoretical study of metal hollow spheres material prepared by this method, No reports at home and abroad, nor related patents.

发明内容 SUMMARY

[0005] 本发明所要解决的技术问题在于针对上述现有技术中的不足,提供一种设计合理、工艺简单、操作步骤简便且生产成本低廉的金属空心球的粉末冶金制备方法。 [0005] The present invention solves the technical problem that the prior art in view of the above deficiencies, to provide a reasonable design, simple process, the production steps and simple low cost method for preparing a metal hollow sphere powder metallurgy.

[0006] 为解决上述技术问题,本发明米用的技术方案是:一种金属空心球的粉末冶金制备方法,其特征在于,该方法包括以下步骤: [0006] To solve the above technical problem, the technical solution of the present invention is used Mingmi: Preparation of powder metallurgy metal hollow spheres, characterized in that the method comprises the steps of:

[0007] 步骤一、将金属粉末与粘合剂溶液混合,经机械搅拌均匀后配制成悬浮液一,之后将消泡剂加入所述悬浮液一中并搅拌均匀得到浆料一;所述粘合剂溶液中粘合剂的质量浓度为O. 1%〜1% ;所述悬浮液一的固含量为5%〜20% ;所述消泡剂的加入量为所述悬浮一重量的O. 1%〜O. 3% ; [0007] Step a, the metal powder mixed with a binder solution, mechanically stirred uniformly formulated as a suspension, after which a defoamer is added to the suspension and stirred uniformly to obtain a slurry; the visco mass concentration of the binder solution is a mixture O. 1% ~1%; the solids content of a suspension of a 5-20%; the amount of defoaming agent added is a weight of the suspension O .. 1% ~O 3%;

[0008] 步骤二、将聚苯乙烯球装入离心模具中,再将步骤一中所述浆料一倒入所述离心磨具中,之后将离心模具装在离心机上进行离心,最后将离心后的聚苯乙烯球随离心模具放在鼓风式烘箱中进行干燥;所述浆料一的倒入量应使离心模具中的聚苯乙烯球被完全覆盖; [0008] Step two, the polystyrene spheres loaded centrifugal mold, then a step in the slurry is poured into the centrifugal a grinder, then centrifuged die mounted on the centrifuge was centrifuged, and finally centrifuged after centrifugation with polystyrene spheres in a mold blast oven dried; the amount of the slurry was poured into a centrifuge should polystyrene beads are completely covered by the mold;

[0009] 步骤三、将金属粉末与粘合剂溶液混合,经机械搅拌均匀后配制成悬浮液二,之后将消泡剂加入所述悬浮液二中并搅拌均匀得到浆料二;所述粘合剂溶液中粘合剂的质量浓度为5%〜15% ;所述悬浮液二的固含量为30%〜60% ;所述消泡剂的加入量为所述悬浮液二重量的O. 1%〜O. 3% ; [0009] Step three, the metal powder mixed with a binder solution, mechanically stirred suspension uniformly formulated as two, then defoamer added to the two suspension and stirred to give a uniform slurry II; the visco mass concentration of the binder solution is a mixture of 5% ~ 15%; the two solids content of the suspension is 30% ~ 60%; the amount of defoaming agent by weight of the two suspension O. . 1% ~O 3%;

[0010] 步骤四、将步骤三中所述浆料二倒入步骤二中干燥后的离心模具中,之后将所述离心模具装在离心机上进行离心,最后将离心后的聚苯乙烯球随离心模具放在鼓风式烘箱中进行干燥;所述浆料二的倒入量应使离心模具中的聚苯乙烯球被完全覆盖; [0010] Step 4 centrifuged mold after step 3 the slurry was poured into two drying step two, after the centrifugal molds mounted on the centrifuge was centrifuged, and finally after centrifugation with polystyrene spheres centrifugal blast mold placed in a drying oven; the amount of the slurry was poured into two centrifuge should polystyrene beads are completely covered by the mold;

[0011] 步骤五、将聚苯乙烯球从步骤四中干燥后的离心模具中取出,包埋于氧化铝填料中放在真空炉中进行热解、烧结,得到金属空心球。 [0011] Step 5 The polystyrene ball was removed from the mold after centrifugation was dried in the Step 4, embedded in an alumina filler material placed in a vacuum oven pyrolyzed and sintered to obtain a metal hollow spheres.

[0012] 上述的一种金属空心球的粉末冶金制备方法,其特征在于,步骤一中所述金属粉末的平均粒度不大于48 μ m,步骤一中所述金属粉末为不锈钢粉末、钛合金粉末、镍基合金粉末、镍粉或Fe-Al金属间化合物粉末;步骤三中所述金属粉末与步骤一中所述金属粉末为同种金属粉末;步骤三中所述金属粉末的粒度与步骤一中所述金属粉末的粒度相同。 Preparation of [0012] the above-described metal powder metallurgy hollow spheres, wherein a mean particle size of the step in the metal powder is not larger than 48 μ m, the step in the metal powder is a stainless steel powder, titanium powder , between the nickel-based alloy powder, nickel powder or powder of Fe-Al intermetallic compound; step three in the metal powder and the metal powder in the step of a same kind of metal powder; step three in the metal powder particle size and a step the same size of the metal powder.

[0013] 上述的一种金属空心球的粉末冶金制备方法,其特征在于,步骤一和步骤三中所述粘结剂溶液为聚乙烯醇溶液、聚乙二醇溶液或羧甲基纤维素溶液。 Preparation of [0013] the above-described metal powder metallurgy hollow spheres, characterized in that said three steps one and a binder solution is a solution of polyvinyl alcohol, polyethylene glycol, carboxymethyl cellulose solution, or a solution of .

[0014] 上述的一种金属空心球的粉末冶金制备方法,其特征在于,步骤一和步骤三中所述消泡剂为正辛醇、聚醚消泡剂或磷酸三丁酯,所述聚醚消泡剂为GP型聚醚消泡剂、GPE型聚醚消泡剂或PPE型聚醚消泡剂。 Preparation of [0014] the above-described metal powder metallurgy hollow spheres, characterized in that, in steps one and three of the defoaming agent is n-octanol, or tributyl phosphate antifoaming polyethers, the poly GP polyether ether antifoams defoamers, GPE defoamer polyether or polyether PPE defoamer.

[0015] 上述的一种金属空心球的粉末冶金制备方法,其特征在于,步骤二中所述聚苯乙烯球的粒度不大于4_。 Preparation of [0015] the above-described metal powder metallurgy hollow spheres, characterized in that, in step two of the polystyrene ball size not greater than 4_.

[0016] 上述的一种金属空心球的粉末冶金制备方法,其特征在于,步骤二和步骤四中所述离心的时间为20min〜200min,所述离心机的转速为2000r/min〜5000r/min ;所述干燥的温度为60°C〜90°C,所述干燥的时间为8h〜24h。 Preparation of [0016] the above-described metal powder metallurgy hollow spheres, characterized in that steps two and four steps of the centrifugation time is 20min~200min, said centrifuge speed of 2000r / min~5000r / min ; the drying temperature of 60 ° C~90 ° C, the drying time is 8h~24h.

[0017] 上述的一种金属空心球的粉末冶金制备方法,其特征在于,步骤五中所述热解、烧结的制度为:以l°c /min〜10°C /min的升温速率将炉内温度升至150°C〜250°C时保温30min〜90min,之后升至300°C〜400°C时保温60min〜120min,然后升至450°C〜550°C时保温30min〜90min,最后升至步骤一中所述金属粉末O. 5〜O. 9倍熔点温度时保温120min〜180min,之后随炉冷却。 Preparation of [0017] the above-described metal powder metallurgy hollow spheres, characterized in that said pyrolysis step 5, sintering system as: temperature increasing rate of l ° c / min~10 ° C / min in the furnace when the heat insulation 30min~90min 60min~120min insulation when the temperature was raised within 30min~90min 150 ° C~250 ° C, then raised to 300 ° C~400 ° C, then raised to 450 ° C~550 ° C, and finally a step of heat 120min~180min raised when said metal powder is O. 5~O. 9 times the melting temperature, then cooling with the furnace.

[0018] 本发明与现有技术相比具有以下优点: [0018] The present invention and the prior art has the following advantages:

[0019] I、本发明制备方法设计合理、工艺简单、操作步骤简便且生产成本低廉。 [0019] I, the present invention has reasonable design method of preparation, the process is simple, easy operation and low cost of production steps.

[0020] 2、本发明制备方法适用于各种金属空心球的制备,采用本发明制备方法制备的金属空心球具有球壳壁厚均匀、光滑、完整,球体尺寸易选择,整体结构易控制等优点。 [0020] 2. Preparation method of the present invention suitable for the preparation of hollow spheres in a variety of metal, metal hollow spheres produced by the production method of the present invention having a spherical shell of uniform thickness, a smooth, complete, easy to select a sphere size, easy to control the overall configuration advantage.

[0021] 下面通过实施例,对本发明的技术方案做进一步的详细描述。 [0021] The following examples, further detailed description of the technical solution of the present invention.

具体实施方式 Detailed ways

[0022] 实施例I [0022] Example I

[0023] 步骤一、将平均粒度为25 μ m的316L不锈钢粉末与质量浓度为O. 5%的羧甲基纤维素溶液混合,经机械搅拌均匀后配制成悬浮液一,之后将正辛醇加入所述悬浮液一中并搅拌均匀得到浆料一;所述悬浮液一的固含量为20% ;所述正辛醇的加入量为所述悬浮一重量的O. 1% ; [0023] Step a, the mixed solution of carboxymethyl cellulose with a mass concentration of 316L stainless steel powder of an average particle size of 25 μ m is O. 5% of, after mechanical stir formulated as a suspension, after which the n-octanol the suspension was added and stirred uniformly to obtain a slurry of a; the suspension a solids content of 20%; the addition amount of n-octanol to the weight of a suspension O. 1%;

[0024] 步骤二、将粒度为3mm的聚苯乙烯球装入离心模具中,再将步骤一中所述浆料一倒入所述离心模具中,之后将离心模具装在离心机上进行离心,最后将离心后的聚苯乙烯球随离心模具放在鼓风式烘箱中进行干燥;所述浆料一的倒入量应使离心模具中的聚苯乙烯球被完全覆盖;所述离心的时间为20min,所述离心机的转速为4000r/min ;所述干燥的温度为60°C,所述干燥的时间为8h ; [0024] Step two, the particle size of the polystyrene spheres centrifuged 3mm charged into a centrifugal mold, then a step in the slurry is poured into a mold in the centrifugal, then centrifuged die mounted on the centrifuge, Finally, after centrifugation of polystyrene balls were dried in the mold with centrifugal blast oven; the amount of the slurry was poured into a centrifuge should polystyrene beads are completely covered by the mold; the centrifugal time to 20min, the centrifuge speed of 4000r / min; the drying temperature of 60 ° C, the drying time is 8H;

[0025] 步骤三、将平均粒度为25 μ m的316L不锈钢粉末与质量浓度为10%的聚乙烯醇溶液混合,经机械搅拌均匀后配制成悬浮液二,之后将磷酸三丁酯加入所述悬浮液二中并搅拌均匀得到浆料二;所述悬浮液二的固含量为50% ;所述磷酸三丁酯的加入量为所述悬浮液二重量的O. 2% ; [0025] Step three, the mixed polyvinyl alcohol solution and the concentration of 316L stainless steel powder of an average particle size of 25 μ m is 10%, after mechanically stirred suspension uniformly formulated as two, after the addition of tributyl phosphate two suspension and stirred to obtain a uniform slurry II; II the suspension a solids content of 50%; the amount of tributyl phosphate is O. 2% by weight of the two suspension;

[0026] 步骤四、将步骤三中所述浆料二倒入步骤二中干燥后的离心模具中,之后将所述离心模具装在离心机上进行离心,最后将离心后的聚苯乙烯球随离心模具放在鼓风式烘箱中进行干燥;所述浆料二的倒入量应使离心模具中的聚苯乙烯球被完全覆盖;所述离心的时间为20min,离心机的转速为4000r/min ;所述干燥的温度为60°C,所述干燥的时间为12h ; [0026] Step 4 centrifuged mold after step 3 the slurry was poured into two drying step two, after the centrifugal molds mounted on the centrifuge was centrifuged, and finally after centrifugation with polystyrene spheres centrifugal blast mold placed in a drying oven; the amount of the slurry was poured into two centrifuge should polystyrene beads are completely covered by the mold; the centrifugation time is 20min, centrifuge speed of 4000r / min; the drying temperature of 60 ° C, the drying time is 12h;

[0027] 步骤五、将聚苯乙烯球从步骤四中干燥后的离心模具中取出,包埋于氧化铝填料中放在真空炉中进行热解、烧结,得到金属空心球;所述热解、烧结的制度为:以l°c /min的升温速率将炉内温度升至200 V时保温30min,之后升至350°C时保温60min,然后升至500°C时保温30min,最后升至步骤一中所述316L不锈钢粉末O. 9倍熔点温度时保温120min,之后随炉冷却。 [0027] Step 5 The polystyrene ball was removed from the mold after the step of drying the centrifugal Fourth, embedded in the alumina filler in a vacuum oven pyrolyzed and sintered to obtain a metal hollow spheres; the pyrolysis sintering system is: for 30min when the temperature increasing rate of l ° c / min in the furnace temperature was raised to 200 V, when incubated for 30min after 60min, was raised to 350 ° C, then raised to 500 ° C, and finally raised to a step of 316L stainless steel powder in the insulation 120min O. 9 times the melting temperature, then cooling with the furnace.

[0028] 实施例2 [0028] Example 2

[0029] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤二中聚苯乙烯球的粒度为3mm和4mm。 [0029] Example embodiments of the present method of preparing the same method of Example I, except that wherein: step two polystyrene spheres particle size is 3mm and 4mm.

[0030] 实施例3 [0030] Example 3

[0031] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤二中聚苯乙稀球的粒度为2mm、3mm、3. 5mm和4mm。 [0031] Example embodiments of the present method of preparing the same method of Example I, except that wherein: a particle size in the two steps of polystyrene balls 2mm, 3mm, 3 5mm and 4mm..

[0032] 实施例4 [0032] Example 4

[0033] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤一与步骤三中所用金属粉末是平均粒度为48 μ m的316L不锈钢粉末。 [0033] Preparation method of the embodiment according to the present embodiment prepared in the same manner as in Example I, except that wherein: step a and step three metal powder is a stainless steel 316L average particle size of powder 48 μ m.

[0034] 实施例5 [0034] Example 5

[0035] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤三中是将平均粒度为25 μ m的316L不锈钢粉末与质量浓度为8%的聚乙烯醇溶液混合,经机械搅拌均匀后配制成悬浮液二,之后将GP型聚醚消泡剂加入所述悬浮液二中并搅拌均匀得到浆料二;所述悬浮液二的固含量为40% ;所述GP型聚醚消泡剂的加入量为所述悬浮液二重量的O. 1%。 [0035] Example embodiments of the present preparation in Example I is prepared, except that wherein: step 3 is 316L stainless steel powder and the concentration of 25 μ m average particle size of 8% polyvinyl alcohol solution was mixed , after mechanical stir formulated as two suspension, after which the defoaming agent added to the GP polyether two suspension and stirred uniformly to obtain slurry II; the two solids content of the suspension was 40%; the GP polyether added in an amount of defoamer by weight of the two suspension O. 1%.

[0036] 实施例6 [0036] Example 6

[0037] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤三中是将平均粒度为25 μ m的304L不锈钢粉末与质量浓度为5%的聚乙二醇溶液混合,经机械搅拌均匀后配制成悬浮液二,之后将GPE型聚醚消泡剂加入所述悬浮液二中并搅拌均匀得到浆料二;所述悬浮液二的固含量为30% ;所述GPE型聚醚消泡剂的加入量为所述悬浮液二重量的O. 3%ο[0038] 实施例7 [0037] Example embodiments of the present preparation in Example I is prepared, except that wherein: step 3 is 304L stainless steel powder with a concentration of 25 μ m average particle size of a 5% solution of polyethylene glycol were mixed mechanically stirred suspension was formulated as two uniform, after which the defoaming agent added to the GPE polyether two suspension and stirred uniformly to obtain slurry II; two solids content of the suspension is 30%; the GPE amount of said polyether-type defoaming agent to the weight of the two suspension O. 3% ο [0038] Example 7

[0039] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤二中聚苯乙烯球的粒度为3mm和4mm ;步骤三中是将平均粒度为35 μ m的316L不锈钢粉末与质量浓度为8%的聚乙烯醇溶液混合,经机械搅拌均匀后配制成悬浮液二,之后将PPE型聚醚消泡剂加入所述悬浮液二中并搅拌均匀得到浆料二;所述悬浮液二的固含量为60% ;所述PPE型聚醚消泡剂的加入量为所述悬浮液二重量的O. 1%。 [0039] In the present embodiment the method of Example I in Example production method, except that wherein: step two polystyrene spheres particle size is 3mm and 4mm; Step three is the average particle size of 35 μ m in 316L stainless steel powder mixed with a polyvinyl alcohol solution concentration of 8% by mass, even after mechanically stirred suspension is formulated into two, then the PPE polyether defoaming agent is added to the two suspension and stirred to give a uniform slurry II; the two solids content of the suspension was 60%; the addition amount of the PPE polyether defoamers O. 1% by weight of the two suspension.

[0040] 实施例8 [0040] Example 8

[0041] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤二中聚苯乙烯球的粒度为3mm和4mm ;步骤三中是将平均粒度为25 μ m的316L不锈钢粉末与质量浓度为5%的聚乙烯醇溶液混合,经机械搅拌均匀后配制成悬浮液二,之后将正辛醇加入所述悬浮液二中并搅拌均匀得到浆料二;所述悬浮液二的固含量为30% ;所述正辛醇的加入量为所述悬浮液二重量的O. 3%。 [0041] A method of the present embodiment in Example I are prepared, wherein except that: the step size of the polystyrene spheres II 3mm and 4mm; Step three is the average particle size of 25 μ m in 316L stainless steel powder mixed with a solution of polyvinyl alcohol concentration of 5% by mass, even mechanically stirred suspension formulated as two, then the octanol was added to the suspension and stirred uniformly to obtain two slurry II; the suspension two solids content of 30%; the addition amount of n-octanol is O. 3% by weight of the two suspension. [0042] 实施例9 [0042] Example 9

[0043] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤一与步骤三中所用金属粉末是平均粒度为25 μ m的FeCrAl合金粉末。 [0043] Preparation method of the embodiment according to the present embodiment prepared in the same manner as in Example I, except that wherein: step a and step three metal powder having an average particle size of 25 μ m of FeCrAl alloy powder.

[0044] 实施例10 [0044] Example 10

[0045] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤一与步骤三中所用金属粉末是平均粒度为25 μ m的TC4钛合金粉末。 [0045] Example embodiments of the present method of preparing the same method of Example I, except that wherein: step a and step three metal powder having an average particle size of 25 μ m to TC4 titanium alloy powder.

[0046] 实施例11 [0046] Example 11

[0047] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤一与步骤三中所用金属粉末是平均粒度为25 μ m的镍铬铝合金粉末。 [0047] Example embodiments of the present method of preparing the same method of Example I, except that wherein: step a and step three metal powder having an average particle size of 25 μ m of nickel-chromium alloy powder.

[0048] 实施例12 [0048] Example 12

[0049] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤一与步骤三中所用金属粉末是平均粒度为25 μ m的镍铬合金粉末;步骤五中热解、烧结的制度为:以TC /min的升温速率将炉内温度升至150°C时保温90min,之后升至300°C时保温120min,然后升至450°C时保温90min,最后升至步骤一中所述金属粉末O. 7倍熔点温度时保温120min。 [0049] The production method according to the present embodiment in Example I are prepared, wherein except that: step a and step three metal powder having an average particle size of 25 μ m of nickel-chromium alloy powder; Fifth pyrolysis step sintering system are: temperature increasing rate of TC / min in the furnace temperature was raised to 150 ° C when incubated 90min, then raised to 300 ° C when incubated 120min, then raised to 450 ° C when incubated 90min, and finally raised to step the metal powder in a heat O. 120min 7 times the melting temperature.

[0050] 实施例13 [0050] Example 13

[0051] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤一与步骤三中所用金属粉末是平均粒度为25 μ m的镍铬合金粉末,步骤三中是将平均粒度为25 μ m的镍铬合金粉末与质量浓度为15%的聚乙烯醇溶液混合,经机械搅拌均匀后配制成悬浮液二,之后将正辛醇加入所述悬浮液二中并搅拌均匀得到浆料二;所述悬浮液二的固含量为40%,所述正辛醇的加入量为所述悬浮液二重量的O. 3% ;步骤五中热解、烧结的制度为:以5°C /min的升温速率将炉内温度升至250°C时保温60min,之后升至400°C时保温90min,然后升至550°C时保温60min,最后升至步骤一中所述金属粉末O. 8倍熔点温度时保温120min。 [0051] The present method of Example embodiment in Example preparation I, wherein except that: step a and step three metal powder having an average particle size of 25 μ m of nickel-chromium alloy powder, in step three is nickel-chromium alloy powder mixed with a concentration of 15 mass% polyvinyl alcohol solution, an average particle size of 25 μ m, after mechanically stirred suspension was formulated as two uniform, after which the suspension was added n-octanol and stir two a slurry II; two solids content of the suspension was 40%, the amount of n-octanol was added to the two suspension weight O. 3%; pyrolysis step 5, sintering system were as follows: when incubated heating rate 5 ° C / min in the furnace temperature was raised to 250 ° C 60min, 90min incubation time was raised after 400 ° C, and then for 60min when raised to 550 ° C, a final step in the metal was raised to incubation at 120min O. 8 times the melting point of the powder.

[0052] 实施例14 [0052] Example 14

[0053] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤一与步骤三中所用金属粉末是平均粒度为25 μ m的镍铬合金粉末,步骤三中是将平均粒度为25 μ m的镍铬合金粉末与质量浓度为5%的聚乙烯醇溶液混合,经机械搅拌均匀后配制成悬浮液二,之后将正辛醇加入所述悬浮液二中并搅拌均匀得到浆料二;所述悬浮液二的固含量为30%,所述正辛醇的加入量为所述悬浮液二重量的O. 2% ;步骤五中热解、烧结的制度为:以10°C /min的升温速率将炉内温度升至200°C时保温30min,之后升至350°C时保温60min,然后升至500°C时保温30min,最后升至步骤一中所述金属粉末O. 5倍熔点温度时保温120min。 [0053] The production method according to the present embodiment in Example I are prepared, wherein except that: step a and step three metal powder having an average particle size of 25 μ m of nickel-chromium alloy powder, step 3 is mixing polyvinyl alcohol solution 25 μ m average particle size of the alloy powder of Ni - Cr concentration of 5%, after mechanically stirred suspension was formulated as two uniform, after which the suspension was added n-octanol and stir two a slurry II; two solids content of the suspension was 30%, the amount of n-octanol was added to the two suspension weight O. 2%; pyrolysis step 5, sintering system were as follows: when incubated for 30min 30min, heating rate 10 ° C / min in the furnace temperature was raised to 200 ° C, for 60min when raised after 350 ° C, then raised to 500 ° C, a final step in the metal was raised to O. 5 120min incubation times when the melting point of the powder.

[0054] 实施例15 [0054] Example 15

[0055] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤一与步骤三中所用金属粉末是平均粒度为25 μ m的镍粉,步骤五中所述热解、烧结的制度为:以8V /min的升温速率将炉内温度升至200°C时保温30min,之后升至350°C时保温60min,然后升至500°C时保温30min,最后升至步骤一中所述金属粉末O. 6倍熔点温度时保温120mino [0056] 实施例16 [0055] Example embodiments of the present preparation in Example I is prepared, except that wherein: step a and step three metal powder having an average particle size of 25 μ m of nickel powder, the pyrolysis step 5 , sintered system as: heat insulation when the temperature increasing rate of 8V / min in the furnace temperature was raised to 200 ° C 30min, then raised to 350 ° C during 60min, and then for 30min when raised to 500 ° C, raised to the final step a thermal insulation in the metal powder O. 120mino [0056] 6 times the melting temperature of Example 16

[0057] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤一与步骤三中所用金属粉末是平均粒度为25 μ m的镍粉,步骤三中是将平均粒度为25 μ m的镍铬合金粉末与质量浓度为8%的聚乙烯醇溶液混合,经机械搅拌均匀后配制成悬浮液二,之后将正辛醇加入所述悬浮液二中并搅拌均匀得到浆料二;所述悬浮液二的固含量为40%,所述正辛醇的加入量为所述悬浮液二重量的O. 2% ;步骤五中热解、烧结的制度为:以6°C /min的升温速率将炉内温度升至200 V时保温30min,之后升至350°C时保温60min,然后升至500°C时保温30min,最后升至步骤一中所述金属粉末O. 9倍熔点温度时保温120min。 [0057] The present method of Example embodiment same as in Example I are prepared, wherein except that: step a and step three metal powder having an average particle size of 25 μ m of nickel powder, step three is the average particle size mixing polyvinyl alcohol solution with a concentration of an alloy of nickel chromium powder 25 μ m was 8%, mechanically stirred suspension uniformly formulated as two, then the octanol was added to the suspension and stirred uniformly to obtain a two slurry two materials; the two solids content of the suspension was 40%, the amount of n-octanol was added O. 2% by weight of the two suspension; pyrolysis step 5, sintering system were as follows: 6 ° when incubated for 30min 60min 30min incubation time when the heating rate C / min in the furnace temperature was raised to 200 V, then raised to 350 ° C, then raised to 500 ° C, in a final step raised to the metal powder O. 9 120min incubation times melting point temperature.

[0058] 实施例17 [0058] Example 17

[0059] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤一与步骤三中所用金属粉末是平均粒度为25 μ m的镍粉,步骤三中是将平均粒度为25 μ m的镍铬合金粉末与质量浓度为5%的聚乙烯醇溶液混合,经机械搅拌均匀后配制成悬浮液二,之后将正辛醇加入所述悬浮液二中并搅拌均匀得到浆料二;所述悬浮液二的固含量为30%,所述正辛醇的加入量为所述悬浮液二重量的O. 1% ;步骤五中热解、烧结的制度为:以1°C /min的升温速率将炉内温度升至200°C时保温30min,之后升至350°C时保温60min,然后升至500°C时保温30min,最后升至步骤一中所述金属粉末O. 8倍熔点温度时保温120min。 [0059] The production method according to the present embodiment in Example I are prepared, wherein except that: step a and step three metal powder having an average particle size of 25 μ m of nickel powder, step 3 is the average particle size mixing polyvinyl alcohol solution with a concentration of an alloy of nickel chromium powder 25 μ m to 5%, mechanically stirred suspension uniformly formulated as two, then the octanol was added to the suspension and stirred uniformly to obtain a two slurry two materials; the two solids content of the suspension was 30%, the amount of n-octanol was added to the two suspension weight O. 1%; pyrolysis step 5, sintering system were as follows: 1 ° when incubated for 30min 30min when the heating rate C / min in the furnace temperature was raised to 200 ° C, for 60min when raised after 350 ° C, then raised to 500 ° C, in a final step raised to the metal powder O incubation at 120min. 8 times the melting temperature.

[0060] 实施例18 [0060] Example 18

[0061] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤一与步骤三中所用金属粉末是平均粒度为25 μ m的316L不锈钢粉末,步骤一中是将平均粒度为25 μ m的316L不锈钢粉末与质量浓度为1%的聚乙烯醇溶液混合,经机械搅拌均匀后配制成悬浮液一,之后将磷酸三丁酯加入所述悬浮液一中并搅拌均匀得到浆料一;所述悬浮液一的固含量为5%,所述磷酸三丁酯的加入量为所述悬浮液一重量的O. 1%。 [0061] The present method of Example embodiment same as in Example I are prepared, wherein except that: step a and step three metal powder having an average particle size of 316L stainless steel powder 25 μ m, the step a is an average 316L stainless steel powder with a particle size concentration of 25 μ m was mixed in a 1% polyvinyl alcohol solution, mechanically stirred uniformly formulated into a suspension, after which the tributyl phosphate is added to the suspension and stirred uniformly to obtain a a slurry; the suspension a solids content of 5%, the amount of tributyl phosphate is O. 1% by weight of said suspension a. .

[0062] 实施例19 [0062] Example 19

[0063] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤一与步骤三中所用金属粉末是平均粒度为25 μ m的镍铬合金粉末,步骤一中是将平均粒度为 [0063] The production method according to the present embodiment and the same method of Example I, wherein except that: step a and step three metal powder having an average particle size of 25 μ m of nickel-chromium alloy powder, step one is The average particle size

25 μ m的镍铜合金粉末与质量浓度为O. 5%的聚乙二醇溶液混合,经机械搅拌均匀后配制成悬浮液一,之后将GP型聚醚消泡剂加入所述悬浮液一中并搅拌均匀得到浆料一;所述悬浮液一的固含量为20%,所述GP型聚醚消泡剂的加入量为所述悬浮液一重量的O. 1%。 Polyethylene glycol solution mixed nickel-copper alloy powder with a mass concentration of 25 μ m is O. 5%, mechanically stirred uniformly formulated as a suspension, after which the GP polyether suspension was added a defoaming agent and stirred uniformly to obtain a slurry; the suspension a solids content of 20%, an amount of the added polyether defoamers GP O. 1% by weight of a said suspension.

[0064] 实施例20 [0064] Example 20

[0065] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤二和步骤四中离心机的转速为5000r/min,离心的时间为20min,干燥的温度为80°C,干燥的时间为18h。 [0065] Example embodiments of the present preparation in Example I is prepared, except that wherein: Fourth centrifuge step and two step speed of 5000r / min, centrifugation time was 20min, the drying temperature is 80 ° C, the drying time was 18h.

[0066] 实施例21 [0066] Example 21

[0067] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤二和步骤四中离心机的转速为2000r/min,离心的时间为200min,干燥的温度为60°C,干燥的时间为24h。 [0067] Example embodiments of the present preparation in Example I are prepared, wherein except that: the centrifuge steps two and four steps of speed of 2000r / min, 200min centrifugation time, the drying temperature is 60 ° C, the drying time was 24h.

[0068] 实施例22 [0069] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤二和步骤四中离心机的转速为3000r/min,离心的时间为lOOmin,干燥的温度为90°C,干燥的时间为8h。 [0068] Example 22 [0069] Example embodiment of the present method for preparing the same as in Example I is prepared, except that wherein: Fourth centrifuge step and two step speed of 3000r / min, centrifugation time lOOmin, drying temperature of 90 ° C, drying time of 8h.

[0070] 实施例23 [0070] Example 23

[0071] 本实施例制备方法与实施例I的制备方法相同,其中不同之处在于:步骤二和步骤四中离心机的转速为4000r/min,离心的时间为60min,干燥的温度为70°C,干燥的时间为24h。 [0071] Example embodiments of the present preparation in Example I is prepared, except that wherein: Fourth centrifuge step and two step speed of 4000r / min, centrifugation time was 60min, the drying temperature is 70 ° C, the drying time was 24h.

[0072] 以上所述,仅是本发明的较佳实施例,并非对本发明作任何限制,凡是根据本发明技术实质对以上实施例所作的任何简单修改、变更以及等效变化,均仍属于本发明技术方案的保护范围内。 [0072] The above, only the preferred embodiment of the present invention, the present invention does not impose any restrictions on who simply any modification made to the technical spirit of the present invention to the above embodiments, changes and equivalent variations as would fall present within the scope of the technical solution of the present invention.

Claims (7)

  1. 1. 一种金属空心球的粉末冶金制备方法,其特征在于,该方法包括以下步骤: 步骤一、将金属粉末与粘合剂溶液混合,经机械搅拌均匀后配制成悬浮液一,之后将消泡剂加入所述悬浮液一中并搅拌均匀得到浆料一;所述粘合剂溶液中粘合剂的质量浓度为O. 1%〜1% ;所述悬浮液一的固含量为5%〜20% ;所述消泡剂的加入量为所述悬浮液一重量的O. 1% 〜O. 3% ; 步骤二、将聚苯乙烯球装入离心模具中,再将步骤一中所述浆料一倒入所述离心模具中,之后将离心模具装在离心机上进行离心,最后将离心后的聚苯乙烯球随离心模具放在鼓风式烘箱中进行干燥;所述浆料一的倒入量应使离心模具中的聚苯乙烯球被完全覆盖; 步骤三、将金属粉末与粘合剂溶液混合,经机械搅拌均匀后配制成悬浮液二,之后将消泡剂加入所述悬浮液二中并搅拌均匀得到浆料二;所述粘 1. A method for preparing a metal powder metallurgy hollow spheres, characterized in that the method comprises the following steps: a step, the metal powder mixed with a binder solution, formulated as a suspension and thoroughly mixed by mechanical stirring, after elimination a foaming agent added to the suspension and the resulting slurry was stirred for a uniform; mass concentration of the adhesive binder solution is O. 1% ~1%; the suspension a solids content of 5% ~ 20%; the amount of defoaming agent added is a weight of the suspension O. 1% ~O 3%;. step two, the polystyrene ball was charged centrifugal mold, then as a step said a slurry is poured into the centrifugal mold, then centrifuged die mounted on the centrifuge was centrifuged, and finally after centrifugation of polystyrene balls in the mold with centrifugal blast drying oven; the slurry a the amount to be poured into the mold of polystyrene centrifugal ball is completely covered; step three, the metal powder mixed with a binder solution, after mechanically stirred suspension was formulated as two uniform, after which the defoaming agent two suspension and stirred to obtain a uniform slurry II; the visco 合剂溶液中粘合剂的质量浓度为5%〜15% ;所述悬浮液二的固含量为30%〜60% ;所述消泡剂的加入量为所述悬浮液二重量的O. 1% 〜O. 3% ; 步骤四、将步骤三中所述浆料二倒入步骤二中干燥后的离心模具中,之后将所述离心模具装在离心机上进行离心,最后将离心后的聚苯乙烯球随离心模具放在鼓风式烘箱中进行干燥;所述浆料二的倒入量应使离心模具中的聚苯乙烯球被完全覆盖; 步骤五、将聚苯乙烯球从离心模具中取出,包埋于氧化铝填料中放在真空炉中进行热解、烧结,得到金属空心球。 Mass concentration of the binder solution is a mixture of 5% ~ 15%; the two solids content of the suspension is 30% ~ 60%; the amount of defoaming agent by weight of the two suspension O. 1 .% ~O 3%; step four, the mold was centrifuged in a two step slurry was poured into three said drying step two, after the centrifugal molds mounted on the centrifuge was centrifuged, and finally after centrifugation poly with the mold in a centrifugal ball styrene blast oven dried; the amount of the slurry was poured into two centrifuge should polystyrene beads are completely covered by the mold; step 5 the polystyrene balls from the centrifuge mold removed, placed in an alumina filler material embedded vacuum oven pyrolyzed and sintered to obtain a metal hollow spheres.
  2. 2.根据权利要求I所述的一种金属空心球的粉末冶金制备方法,其特征在于,步骤一中所述金属粉末的平均粒度不大于48 μ m,步骤一中所述金属粉末为不锈钢粉末、钛合金粉末、镍基合金粉末、镍粉或Fe-Al金属间化合物粉末;步骤三中所述金属粉末与步骤一中所述金属粉末为同种金属粉末;步骤三中所述金属粉末的粒度与步骤一中所述金属粉末的粒度相问。 The production method of a metal powder metallurgy I according to claim hollow spheres, wherein a mean particle size of the step in the metal powder is not larger than 48 μ m, the step in the metal powder is a stainless steel powder between titanium alloy powder, a nickel-based alloy powder, nickel powder or powder of Fe-Al intermetallic compound; step 3 and the step of the metal powder in the metal powder is a same kind of metal powder; step 3 the metal powder particle size with a step in the metal powder phase Q.
  3. 3.根据权利要求I所述的一种金属空心球的粉末冶金制备方法,其特征在于,步骤一和步骤三中所述粘合剂溶液为聚乙烯醇溶液、聚乙二醇溶液或羧甲基纤维素溶液。 The production method of a metal powder metallurgy I according to claim hollow spheres, characterized in that said three steps one and the binder solution is a solution of polyvinyl alcohol, polyethylene glycol or carboxymethylcellulose solution methyl cellulose solution.
  4. 4.根据权利要求I所述的一种金属空心球的粉末冶金制备方法,其特征在于,步骤一和步骤三中所述消泡剂为正辛醇、聚醚消泡剂或磷酸三丁酯,所述聚醚消泡剂为GP型聚醚消泡剂、GPE型聚醚消泡剂或PPE型聚醚消泡剂。 The production method of a metal powder metallurgy I according to claim hollow spheres, characterized in that, in steps one and three of the defoaming agent is n-octanol, polyether defoamers, or tributyl phosphate the defoaming agent is a polyether GP polyether defoamers, polyether defoamers or the GPE PPE polyether defoamer.
  5. 5.根据权利要求I所述的一种金属空心球的粉末冶金制备方法,其特征在于,步骤二中所述聚苯乙烯球的粒度不大于4mm。 The production method according to one metal powder metallurgy I according to claim hollow spheres, wherein the particle size of the polystyrene spheres step two is no greater than 4mm.
  6. 6.根据权利要求I所述的一种金属空心球的粉末冶金制备方法,其特征在于,步骤二和步骤四中所述离心的时间为20min〜200min,所述离心机的转速为2000r/min〜5000r/min ;所述干燥的温度为60°C〜90°C,所述干燥的时间为8h〜24h。 The production method of a metal powder metallurgy I according to claim hollow spheres, wherein steps two and four steps of the centrifugation time is 20min~200min, said centrifuge speed of 2000r / min ~5000r / min; the drying temperature of 60 ° C~90 ° C, the drying time is 8h~24h.
  7. 7.根据权利要求I所述的一种金属空心球的粉末冶金制备方法,其特征在于,步骤五所述热解、烧结的制度为:以TC /min〜10°C /min的升温速率将炉内温度升至150°C〜250°C时保温30min〜90min,之后升至300°C〜400°C时保温60min〜120min,然后升至450°C〜550°C时保温30min〜90min,最后升至步骤一中所述金属粉末O. 5〜O. 9倍熔点温度时保温120min〜180min,之后随炉冷却。 The production method of a metal powder metallurgy I according to claim hollow spheres, wherein said five pyrolysis step, as sintering system: temperature increasing rate of TC / min~10 ° C / min will be when the heat insulation 30min~90min 60min~120min when the furnace temperature was raised to heat 30min~90min 150 ° C~250 ° C, then raised to 300 ° C~400 ° C, then raised to 450 ° C~550 ° C, 120min~180min incubated in a final step raised to the metal powder O. 5~O. 9 times the melting temperature, then cooling with the furnace.
CN 201210315834 2012-08-30 2012-08-30 Powder metallurgy fabrication method of hollow metal sphere CN102806355A (en)

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WO2009023697A2 (en) * 2007-08-14 2009-02-19 The Regents Of The University Of California Hollow silica nanospheres and methods of making same
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CN101259402A (en) * 2004-11-11 2008-09-10 中国科学院化学研究所 Method for preparing hollow ball with double-layer structure and hollow ball with multi-layer complex structure by template method
WO2009023697A2 (en) * 2007-08-14 2009-02-19 The Regents Of The University Of California Hollow silica nanospheres and methods of making same
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