TWI465304B - 模料與製造模料的方法 - Google Patents

模料與製造模料的方法 Download PDF

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TWI465304B
TWI465304B TW097131395A TW97131395A TWI465304B TW I465304 B TWI465304 B TW I465304B TW 097131395 A TW097131395 A TW 097131395A TW 97131395 A TW97131395 A TW 97131395A TW I465304 B TWI465304 B TW I465304B
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wax
molding material
polar
polyene
polypropylene
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Eberhard Grath
Wilfried Aichele
Joost Nowak
Josef Arnold
Klaus Czerwinski
Eva Weisser
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Bosch Gmbh Robert
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Description

模料與製造模料的方法
本發明關於一種申請專利範圍第1項引文之利用粉末射出成形方法製造模製體用的模料，此外本發明關於一種製造一種模料，用於利用粉末射出成形方法製造模製體，包含至少一種無機粉末及一種結合劑系統，該結合劑系統至少含有一種聚烯及另外至少一種蠟，當作有機成份。
在粉末射出成形的場合，依所使用無機粉末而定，在金屬粉末射出成形方法和陶瓷粉末射出方法係不同者，在前者的情形係使用金屬當作無機粉末，在後者則用陶瓷。
一種用於模製的結合劑系統(該模料利用金屬粉末射出成形方法加工)舉例而言，見於德專利DE-C 40 33 752除了一種聚合物外，此結合劑系統含有一種低分子成分。適合的低分子成份為環十二烷、環十二烷酮、環十二烷醇或硬脂醯醇。所用聚合物舉例而言為一種較低黏度之改質的聚丙烯，例如在空氣中氧化且在副反應中氧化分解的聚丙烯。
此易揮發的成份與聚烯一同構成一共同之固體溶劑因此呈軟化劑作用。但由於有易揮發成份，此模料，舉例而言，不能用一連續的方法預裹膜(vorkonfektionieren)成顆料，因為當冷卻時一部分易揮發成份蒸發，且以此方式使結合劑系統的組成失控地改變。這種結合劑系統(如DE-C 40 33 952)中所述者)的另一缺點為：只有當結合劑系統中 聚丙烯比例至少60%重量時，才能達成夠高的加工黏度。
在DE-C 196 48 925提到利用粉末射出成形方法製造開放孔隙的模製體，此處所用的模料除了金屬或陶瓷粒子外還含有一種聚醯胺以及軟化劑或蠟，它在模製件成形後可用一溶劑溶解出來，但此處所用的聚醯胺的缺點為：當熱解(Pyolyse)-(它用於將聚醯胺從模製體除去)--的場合時，有很大比例的熱解碳留在模製體孔隙體，它在燒結時會改變合金組成及組織(特別是在顆粒界面)。
本發明關於一種模料，用於利用粉末射出成形方法製造模製體，包含至少一種無機粉末及一種結合劑系統，該結合劑系統至少含有一種聚烯及另外至少一種蠟，其中該至少一種聚烯及/或蠟或二者係極性改質者藉著在模料中使用蠟，舉例而言，模料也可押出成形及顆粒化，其中押出的熔融物流在周圍環繞條件下達成。舉先前技術的低分子成份(它在室溫呈固體溶劑且當溫度升高時容易揮發)不同者，在周圍條件冷卻時，蠟不會揮發。因此模製的組成不會改變。此外，蠟比起環十二烷、環十二烷醇或硬酯醯醇(它一如先前技術的習知的模料當作低分子成份使用)來，在模料加工溫度可造成較高的黏度。由於蠟黏度較高，因此可將較小比的聚醯加到模料。因此，舉例而言，在結合劑系統中可調整一種比例：三分之一的聚醯對三分之二的蠟。當混合比在此範圍時，當製造模製體時，在除去蠟後，得到一具有開放孔隙構成之由金屬或陶瓷粉末及聚烯構成的 模製體，其中，剩餘結合劑(亦即聚烯的熱解物)用熱除去的作業可比在封閉孔隙構造的模製體更快。這點係有可能者，因聚烯的成分比起先前技術的習知模料少，因此還是可能的。由於在先前技術的習知模料的聚烯比例較大，故要除去聚烯所需之熱解時間較久。
因此，舉例而言，本發明的模料含有至少一種未改質的聚烯和一種極性蠟。此外，模料也含有至少一種極性改質的聚烯或一種非極性蠟，或一種極性改質的聚烯和一種極性蠟。此外也可使模料例如含有至少一種未改質的聚烯及至少一種極性改質的聚烯及一至非極性的蠟。最後還可由至少由一種非極性聚烯及至少一種極性蠟及至少一種非極性蠟組合。
藉著使用極性改質的聚烯與極性蠟，可在模料中省卻附加中分散劑例如脂肪酸。先前技術中習知的低分子分解劑一般良好附著在無機粉末表面，但對聚烯呈一種分離劑的形式。使用極性改質的聚烯的優點為：無機粉末在熔融物中保持在分散液中，而不須加分散劑，因為聚合本身呈分散劑作用。由於省卻分散劑，故利用粉末射出成形所製的模製件的脆度減少。
適當的高分子蠟(它們可用於作模料)舉例而言為氧化的聚乙烯蠟用順丁烯二酸酐嫁接的聚乙烯或聚丙烯蠟，呈極性蠟形式。所用非極性蠟的例子可用石蠟、聚乙烯及聚丙烯蠟。
結合劑系統中蠟的比例在40~90重量%範圍。利用結 合劑系統中的蠟，可在加工時調整模料的黏度。由於蠟黏度一般比起在室溫呈固體的有機溶劑更高(如先前技術的模料所用之溶劑)故可將模料中的聚烯比例減少到比先前技術習知的模料更少，由於在聚烯用熱解程序除去之前，該蠟一般可利用溫度處理(或更常用地藉使用溶劑)從一個利用粉末射出成形方法製造的模部件分，因此要利用熱分解去的有機物成份的比例，由於聚烯比例較低，因而較少。因而熱解時間減少，特別是當聚烯比例小得使模製體在除去蠟後呈開放孔隙時尤然。用於作模料使用之可作極性改質的聚烯宜為一種極性改質的聚丙烯或未改質的聚丙烯或二者的組合，聚丙烯可呈均聚物或共聚物的形式存在，且宜呈丙烯乙烯共聚物的形式，其中該均聚物或共聚物可藉氧化嫁接而作極性改質。使用聚丙烯的優點為：它特別是和有大得多的蠟數目的聚醯胺相較，可形成一種固體溶劑，所謂的「玻璃」，此外，可經由該極性改質的聚烯的種類與無機粉末作交換作用，例如嫁接或氧化，或利用極性改質或未改質的聚烯組合而切割。聚丙烯的另一優點為：在保護氣體中作熱解時，留下之碳的殘餘物很小。
舉例而言，極性改質的聚丙烯為用順丁烯二酸酐或(甲基)胺基甲酸嫁接的聚丙烯，此外，該極性改質的聚丙烯也可為一種被氧化的及如此氧化分解的聚丙烯。
舉例而言，氧化的聚丙烯係用習知的聚丙烯類型作捏合(Mastifizieren)而製造。藉著改變分解程度，該聚丙烯及結合劑系統可很容易對不同粒子大小及不同的模製件(它們 要由此模料製造)的無機粉末作配合。氧化作用或氧化分解係在有周圍空氧存在的情形達成。這種反應使得該氧化分解的聚丙烯含極性基團。
如上述，極性改質的聚丙烯的優點為：它將用氧化物皮層包覆的金屬粉末潤化的能力比起具有相同流動指數的未改質聚丙烯更佳。因此可省卻不必添加低分子的潤化輔助劑，極性蠟也促使金屬粉末有較佳的潤化作用。
該模料中所含的至少一種無機粉末一般為一種陶瓷粉末或金屬粉末。
可用於製造模料的適當陶瓷。舉例而言，為氧化鋁、氧化鋯、碳化矽、氮化矽、或碳化鎢。
用於利用粉末射出成形法用在模料中以製造模製體用的金屬，舉例而言，為純鐵、鐵鎳合金、鐵鈷合金、不銹鋼(鉻鋼)，如X65Gr13、鎳鉻鋼、及軟磁鋼。
本發明的模料一般含有50~70體積%範圍的無枌末成份，非極性以及可極性改質的聚烯的比一般總量在10~60重量%範圍，而蠟的比例為40~90重量%範圍(相對於總結合劑比例)，此無極粉末、極性改質的聚烯與蠟的比例係依模料之所要的應用而定。此外該比例和使用的無機粉末，使用之可極性改質的聚烯及使用的蠟有關。
此外本發明關於一種製造該模料的方法。
依本發明的一種製造模料的方法，該種模料，用於利用粉末射出成形方法製造模製體，包含至少一種無機粉末及一種結合劑系統，該結合劑系統至少含有一種聚烯及另 外至少一種蠟，包含以下步驟：(a)將一混合物熔化及均化，由該至少一無機粉末，至少一聚烯及至少一蠟構成，其中至少一聚烯及/或蠟作極性改質，(b)使熔融物模製成形及凝固。
在步驟(a)中，熔化和均化作業宜在一連續的二螺桿揉捏機中或一開放的剪力滾子揉捏機中實施。由於使用蠟及可能省卻了在結合劑系統在常溫呈固態的有機溶劑。故可在開放的大氣中作熔化、均化及冷卻。由於蠟的沸點比有機溶液體溶劑高，故它不會在開放大氣中從融物蒸發或汽化。
在該連續的二螺桿揉捏機或開放的剪力滾子揉捏機中，該無機粉末，至少一種可極性改質的聚烯及至少一種可為極性的蠟作密集的混合。此密集混合使混合物均化。用此方式，該無機粉末均勻地分佈在該熔融物(由至少一種蠟和至少一種聚烯構成)中。
一般利用本發明的方法製造一種中間產物，一般為一種顆料。這點係在步驟(b)中在熔融物形成時達成。但除了製造顆料外，也可在步驟(b)中將模料直接成形而形成所要製的模製部件。但較宜製造一種顆料，它可在隨後的粉末射出成形程序成形成一模製部件。要製造該顆料，係將熔的模料在一配料機(Compounder)的出口經一孔板擠出。熔融物料流係直接在孔板上切斷(熱斷裂)或在一輸送帶上一直冷卻到凝固為止並在冷卻到末端打碎(顆粒化)。
要製造顆料，一般使用該連續式二桿揉捏機當作複合機，模料一般呈擠出的料流形式離開此複合機，該料流在一條輸送帶上在一空氣流中冷卻。藉著用蠟與聚烯，在模料中不含會蒸發的成份。因此在冷卻使在周圍空氣中模料的組成不會改變。
在本發明的方法的一實施例中，在第一步驟，該聚烯在一開放的剪力滾子揉捏機中氧化或用氧化方式分解成一極性改質的聚烯，如果聚烯定量供應到剪力滾子的方式係呈熔融物料流方式從一押出機或熔融物泵出來，則當用開放式剪力滾子揉捏機時就甚有利。這點有一優點，即：不同於習知方式呈顆粒形式量供應，熔融物料流施加的地點可更佳地定義。如此在剪力好揉捏機上的駐留時間分佈曲線寬度也窄得多。此外，由於聚烯呈熔融物方式給出，故可省卻顆粒在剪力滾子揉捏器在熱滾子上熔化的作業。這點使得在同樣通過量的效率時，有效氧化時間更長。
本發明的模料特別適合製造粉末射出成形的模製部件，為此，模料在射出成形機中熔化並注入用於製造模製部件用的模具中。模料在模具中凝固。
在模部件射出成形後，先將結合劑系統除去。為此，先將該至少一種蠟從模製部件除去。舉例而言，這點利用溶劑萃取達成。在此，該玉少一種蠟從複製部件溶出來。
在另一步驟中，一般將未溶解的結合劑成分用熱解除去。在此，結合劑系統的剩餘物一般為在模製部件中所含的不溶的聚烯。在用具一金屬粉末模料作粉末射出成形 時，熱解作用宜在惰性或還原性的大氣中實施，以避免金屬粉末表面氧化。但在用具陶瓷粉末的模料作粉末射出成形程序時，該熱解作用一般在空氣存在的情形達成。因此除了熱分解外，同時還造成氧化。
將結合劑系統除去後，將仍留著的粉末骨架(由金屬或陶瓷粉末構成)燒結成一金屬或陶瓷構件，如果在大氣壓力下燒結時，在組織中產生不容許的尺寸或數目的孔隙，則它們可在較高壓力燒結(壓力燒結)或利用補充之熱等壓(heißisostatisch)方式壓製而大大減少。
由本發明模料製造的模製部件，舉例而言，係為金屬的閥應及閥鐵或磁路元件，它們用於量控制閥中。可由本發明的模料製造的陶瓷構件舉例而言為流動泵的跑動輪。
 [實例1]
由一種模料成形形成模製部件，它含94重量%316L鋼板、3重量%聚丙烯乙烯共聚物[具有3重量%乙烯成份(Total公司的PPR3260)及3重量%一種用順丁二酸酐嫁接的聚丙烯蠟(Clariant公司的Licocene PPMA 1332 T10)，然後將蠟從模製部件除去。為此將它在一Soxhlet中在己烷中在己烷蒸發溫度附件的溫度處理500分鐘。將蠟除去後，將聚烯在氮大氣中利用熱解從模製部件除去。為此，將模製部件先以5℃/每分的速率加熱到37℃。然後將溫度在37℃保持30分。然後用2℃/分溫度上升速率再加熱到450℃，在於450℃保持30分，然後開始燒結程序，以將金屬粉末 燒結成金屬模製部件。
[實例2]
使用一種模料成形形成模製部件，它含94重量%316L鋼板、3重量%聚丙烯乙烯共聚物[具有3重量%乙烯成份(Total公司的PPR3260)(它在混入模料前先氧化或作氧化分解)及3重量%的一種非極性丙烯蠟(Clariant公司的Licocene PP1302)。該氧化或氧化分解的聚丙烯-乙烯共聚物的羥基數為1.2mgKOH/g，酸數為0.3mgKOH/g。蠟與聚烯的除去方式類似於實施例1。
[實例3]
要製造一模製部件，使用一種模料含94重量%的316L鋼粉，3重量%的一種用順丁二酸酐嫁接的乙烯丙烯共聚物(杜邦公司的MZ 203 D)及3重量%的一種非極性聚丙烯共蠟(Clariant公司的Licocene PP 1302)。蠟聚烯除去方式類似於例1與2。

Claims (13)

  1. 一種模料，用於利用粉末射出成形方法製造模製體，包含至少一種無機粉末及一種結合劑系統，該結合劑系統至少含有一種聚烯及另外至少一種蠟，其特徵在：該至少一種聚烯及/或蠟係極性改質者，且該極性改質的聚烯為一種極性改質的聚丙烯。
  2. 如申請專利範圍第1項之模料，其中：該至少一種蠟由以下之物選出：氧化之聚烯蠟、用順丁烯二酸酐嫁接的聚乙烯或聚丙烯蠟、或用(甲基)丙烯酸嫁接的聚乙烯或聚丙烯蠟或其混合物。
  3. 如申請專利範圍第1或第2項之模料，其中：結合系統中中蠟的比例在40~90重量%範圍。
  4. 如申請專利範圍第4項之模料，其中：該極性改質的聚丙烯為用順丁烯二酸酐或(甲基)丙烯酸嫁接的聚丙烯或氧化的或用氧化分解的聚丙烯。
  5. 如申請專利範圍第1或第2項之模料，其中：該無機粉末為一陶瓷粉末或一金屬粉末。
  6. 如申請專利範圍第1或第2項之模料，其中：該無機粉末的比例在50~70體積%範圍，可極性改質的聚烯的比例在10~60重量%範圍，該蠟的比例在結合劑成份的40~90重量%範圍。
  7. 一種製造模料的方法，該種模料，用利用粉末射出成形方法製造模製體，包含至少一種無機粉末及一種結合劑系統，該結合劑系統至少含有一種聚烯及另外至少一種 蠟，包含以下步驟：(a)將一混合物熔化及均化，由該至少一無機粉末，至少一聚烯及至少一蠟構成，其中至少一聚烯及/或蠟作極性改質，(b)使熔融物模製成形及凝固，其中該極性改質的聚烯為一種極性改質的聚丙烯。
  8. 如申請專利範圍第7項之方法，其中：在步驟(a)中，熔融與均化作業在一連續二螺桿揉捏機中實施。
  9. 如申請專利範圍第7或第8項之方法，其中：在步驟(b)中，該熔融物成形時製造一種顆粒。
  10. 如申請專利範圍第7項之方法，其中：在一第一步驟中該聚烯在一開放之剪力滾子揉捏器中氧化或用氧化方式分解成一種極性改質的聚烯。
  11. 如申請專利範圍第10項之方法，其中：聚烯呈熔融物流形式加到剪力滾子。
  12. 一種用於由申請專利範圍第1項的模料製造模製部件的方法，其中該模料成形成一模製體，將蠟從模製體除去，如此形成一開放多孔隙體。
  13. 如申請專利範圍第12項之方法，其中：由該開放多孔隙體利用高溫分解將聚烯除去。
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