CN116217246A - 一种无机粘结剂以及无机粘结剂/TiC复合材料的制备方法 - Google Patents
一种无机粘结剂以及无机粘结剂/TiC复合材料的制备方法 Download PDFInfo
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- CN116217246A CN116217246A CN202310170984.7A CN202310170984A CN116217246A CN 116217246 A CN116217246 A CN 116217246A CN 202310170984 A CN202310170984 A CN 202310170984A CN 116217246 A CN116217246 A CN 116217246A
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- inorganic binder
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- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 5
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- 239000010936 titanium Substances 0.000 description 4
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Abstract
本发明公开了一种无机粘结剂以及无机粘结剂/TiC复合材料的制备方法,该方法包括以下步骤:(1)采用高温熔炼法制备无机粘接剂;(2)无机粘结剂/TiC复合材料成型料的配制;(3)无机粘结剂/TiC复合材料的烧结。通过本发明方法能制备出显微结构均匀致密的无机粘结剂/TiC复合材料,热压烧结后无机粘接剂与TiC粉末界面结合良好,材料抗弯强度能达到200MPa,硬度达到HRC54‑62,在5wt%的盐酸溶液中浸泡24h,材料表面无明显的腐蚀现象,该材料可以在某些酸性环境下作为耐磨材料使用。
Description
技术领域
本发明属于复合材料制备领域,具体是一种无机粘结剂以及无机粘结剂/TiC复合材料的制备方法,尤其涉及一种可应用于酸性环境下的TiC基复合耐磨材料制备的方法。
背景技术
TiC是一种常见的工业用碳化物材料,为灰色金属状面心立方晶格固体,熔点3200℃,沸点4820℃,相对密度4.93g/cm3,莫氏硬度大于9。目前TiC常作为硬质相原料而广泛应用于TiC基钢结合金的工业生产中。TiC基钢结合金中TiC一般占合金总质量的30%-70%,其余部分为作为粘结相的钢基体,常见的钢基体成分有碳钢、合金钢、工具钢、高速钢、高锰钢、耐热钢和不锈钢等。TiC基钢结合金的制备工艺是经过原料粉末混合、压制成型、烧结、锻造、切削加工、热处理等工序后,制备出各种规格、形状的TiC基钢结合金制品。该工艺制备出的TiC基钢结合金材料组织特点是微细的TiC硬质相均匀弥散地分布于钢的基体中,因此TiC基钢结合金兼有TiC的硬度和耐磨性以及钢的良好力学性能,主要用作耐磨零件和机器构件。
TiC自身具有良好的化学稳定性,不溶于盐酸和硫酸,仅溶于王水和氢氟酸,但是TiC基钢结合金由于含有大量的钢基体粘结相,其耐酸性差,造成TiC基钢结合金材料无法应用于酸性工作环境,如耐酸泥浆泵的耐磨内衬等,限制了TiC基复合材料的应用。
发明内容
本发明的目的是为了弥补已有技术中的缺陷,提供了一种无机粘结剂以及无机粘结剂/TiC复合材料的制备方法,该方法制备出的无机粘结剂/TiC复合材料,与传统的钢结合金不同,粘接剂为特殊设计的无机材料,具有良好的耐酸性能,同时复合材料中存在大量的TiC硬质相,具有较高的硬度和耐磨性能,可以应用于酸性环境下的耐磨构件制备。
本发明是通过以下技术方案实现的:
1、一种无机粘结剂,其特征在于:其各原料组分的重量百分比配方如下:
硼酸 5%-8%
氧化铋 10%-15%
碳酸钾 5%-8%
氧化锆 3%-4%
三氧化二铬 3%-4%
三氧化二铁 2%-4%
二氧化硅 57%-72%。
2、根据权利要求其所述的一种无机粘结剂/TiC复合材料的制备方法,其特征在于:依次包括以下步骤:
(1)采用高温熔炼法制备无机粘接剂:
(a) 无机粘接剂的各原料组分的重量百分比配方如下:
将称好的各种原料组分倒入行星式球磨机的刚玉球磨坛中,刚玉球磨坛直径150mm,按球料质量比1-1.4:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球磨球占50%,直径小于10mm的刚玉球磨球占50%。刚玉球磨坛自转速度为350-450r/min,公转速度为100-140 r/min。原料球磨混合30-60min后取出,获得无机粘结剂的熔炼原料料粉;
(b)无机粘结剂的熔炼与破碎
将坩埚炉以2-5℃/min的速度,升温到1430-1450℃,塞上堵料杆,倒入混好的熔炼原料料粉,倒入熔炼原料料粉的体积为坩埚体积的1/2-2/3,在坩埚炉出料口处放一装满水的不锈钢容器;待炉温再次升到1430-1450℃时,保温1-2h,提起堵料杆让熔化的熔炼原料料粉流入水中进行水淬,得到无机粘结剂碎块;
将水淬后的无机粘结剂碎块收集,倒入行星式球磨机的刚玉球磨坛中,加入与无机粘结剂碎块等重的水,球磨坛直径150mm,按球料质量比1-1.4:1的比例加入刚玉球磨球,其中直径为20mm的刚玉球占30% ,直径为10-20mm的刚玉球占70%;球磨坛自转速度为600-800r/min,公转速度为120-150 r/min,无机粘结剂碎块球磨8-12h后得到无机粘结剂浆料,将得到的无机粘结剂浆料倒入盛料盘中;
(c) 无机粘结剂的干燥过筛
将无机粘结剂浆料在110-130℃下干燥,待无机粘结剂浆料完全干透后用塑料铲将其铲起倒入行星式球磨机的刚玉球磨坛中,刚玉球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球磨球占50% ,直径小于10mm的刚玉球磨球占50%;刚玉球磨坛自转速度为400r/min,公转速度为120 r/min,原料球磨2-4h后得到无机粘结剂粉体,将无机粘结剂粉体倒出过350-450#筛,过筛后得到无机粘结剂,将无机粘结剂封袋后放在干燥塔中,待用;
(2)无机粘结剂/TiC复合材料成型料的配制
无机粘结剂/TiC复合材料的各原料组分的重量百分比配方如下:
TiC粉末(直径1-10微米) 70%-80%
无机粘结剂 15%-27%
无水乙醇 3%-5%
将称好的各种原料组分倒入行星式球磨机的刚玉球磨坛中,刚玉球磨坛直径150mm,按球料质量比1-1.4:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球占50% ,直径小于10mm的刚玉球占50%;刚玉球磨坛自转速度为350-450r/min,公转速度为100-140 r/min;原料球磨混合30-60min后取出,获得无机粘结剂/TiC复合材料成型料;
(3)无机粘结剂/TiC复合材料的烧结
根据零件尺寸称取相应重量的无机粘结剂/TiC复合材料成型料,再倒入石墨模具中,并将该石墨模具组装好后,放入热压炉中,在氩气保护气氛下,以5-8℃/min的速度升温至900-950℃,保温30-50min,保温同时施加20-40MPa的成型压力,保温完成后石墨模具带压随炉冷却,当温度低于700℃时,卸除压力同时停止输送氩气,石墨模具继续随炉冷却,当炉温冷却到70℃以下时,开炉打开模具,获得无机粘结剂/TiC复合材料零件成品。
所述的一种无机粘结剂/TiC复合材料的制备方法,其特征在于,依次包括以下步骤:
(1)采用高温熔炼法制备无机粘接剂:
(a) 无机粘接剂的各原料组分的重量百分比配方如下:
硼酸 5%-8%
氧化铋 10%-15%
碳酸钾 5%-8%
氧化锆 3%-4%
三氧化二铬 3%-4%
三氧化二铁 2%-4%
二氧化硅 57%-72%
将称好的各种原料组分倒入行星式球磨机的刚玉球磨坛中,刚玉球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球磨球占50% ,直径小于10mm的刚玉球磨球占50%。刚玉球磨坛自转速度为400r/min,公转速度为120 r/min。原料球磨混合30-60min后取出,获得无机粘结剂的熔炼原料料粉。
(b)无机粘结剂的熔炼与破碎
将坩埚炉以2-5℃/min的速度,升温到1430-1450℃,塞上堵料杆,倒入混好的熔炼原料料粉,倒入熔炼原料料粉的体积为坩埚体积的1/2-2/3,在坩埚炉出料口处放一装满水的不锈钢容器;待炉温再次升到1430-1450℃时,保温1-2h,提起堵料杆让熔化的熔炼原料料粉流入水中进行水淬,得到无机粘结剂碎块。
将水淬后的无机粘结剂碎块收集,倒入行星式球磨机的刚玉球磨坛中,加入与无机粘结剂碎块等重的水,球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为20mm的刚玉球占30% ,直径为10-20mm的刚玉球占70%;球磨坛自转速度为600-800r/min,公转速度为120-150 r/min,无机粘结剂碎块球磨8-12h后得到无机粘结剂浆料,将得到的无机粘结剂浆料倒入盛料盘中。
(c) 无机粘结剂的干燥过筛
将无机粘结剂浆料在120℃下干燥,待无机粘结剂浆料完全干透后用塑料铲将其铲起倒入行星式球磨机的刚玉球磨坛中,刚玉球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球磨球占50% ,直径小于10mm的刚玉球磨球占50%;刚玉球磨坛自转速度为400r/min,公转速度为120 r/min,原料球磨2-4h后得到无机粘结剂粉体,将无机粘结剂粉体倒出过400#筛,过筛后得到无机粘结剂,将无机粘结剂封袋后放在干燥塔中,待用。
(2)无机粘结剂/TiC复合材料成型料的配制
无机粘结剂/TiC复合材料的各原料组分的重量百分比配方如下:
TiC粉末(直径1-10微米) 70%-80%
无机粘结剂 15%-27%
无水乙醇 3%-5%
将称好的各种原料组分倒入行星式球磨机的刚玉球磨坛中,刚玉球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球占50% ,直径小于10mm的刚玉球占50%;刚玉球磨坛自转速度为400r/min,公转速度为120 r/min;原料球磨混合30-60min后取出,获得无机粘结剂/TiC复合材料成型料。
(3)无机粘结剂/TiC复合材料的烧结
根据零件尺寸称取相应重量的无机粘结剂/TiC复合材料成型料,再倒入石墨模具中,并将该石墨模具组装好后,放入热压炉中,在氩气保护气氛下,以5-8℃/min的速度升温至900-950℃,保温30-50min,保温同时施加20-40MPa的成型压力,保温完成后石墨模具带压随炉冷却,当温度低于700℃时,卸除压力同时停止输送氩气,石墨模具继续随炉冷却,当炉温冷却到70℃以下时,开炉打开模具,获得无机粘结剂/TiC复合材料零件成品。
下面对本发明作进一步解释:
(1)采用高温熔炼法制备无机粘接剂:
无机粘接剂的重量百分比配方如下:
硼酸 5%-8%
氧化铋 10%-15%
碳酸钾 5%-8%
二氧化锆 3%-4%
三氧化二铬 3%-4%
三氧化二铁 2%-4%
二氧化硅 57%-72%
该配方的无机粘接剂在1430-1450℃高温熔炼后,形成的为SiO2-Bi2O3-B2O3-K2O系玻璃材料,其中SiO2提供的硅氧四面体为玻璃网络的主要组成体。Bi2O3的加入会向玻璃网络结构中提供铋氧八面体,可以大幅度降低玻璃材料的软化点。粘结剂中H3BO3和K2CO3的同时加入,在无机粘接剂熔炼过程中,H3BO3会转变为B2O3, K2CO3转变为K2O,K2O向B2O3提供自由氧,使硼氧三角体转变为硼氧四面体进入到玻璃结构中,在保证B2O3对玻璃的促熔效果的前提下还不会大幅度降低玻璃的稳定性和力学性能。综上所述无机粘接剂中按比例加入SiO2、Bi2O3、H3BO3和K2CO3等主要原料,通过熔炼可以形成软化点较低的稳定的SiO2-Bi2O3-B2O3-K2O系玻璃材料。
无机粘接剂中加入少量的ZrO2,Zr4+存在于粘接剂玻璃网络结构的空隙中,对玻璃网络中的O2-产生较强的极化作用,可以提高粘接剂的耐酸性;Cr2O3的加入能够降低粘接剂熔融状态时的表面张力,使粘接剂更好的润湿TiC粉末;粘接剂中加入Fe2O3能促进在热压烧结过程中TiC表面的Ti原子与无机粘接剂形成Ti-O-Fe键(参见图1、图2)。图1为原料TiC粉末的钛元素XPS分析,其中458.9ev处的Ti2p3/2峰和464.8eV处的Ti2p1/2峰对应于Ti4+,主要来源于TiC;457.3eV处的Ti2p3/2峰463.3eV处的Ti2p1/2峰对应于Ti3+,主要来源TiC表面的Ti2O3氧化膜。图2为烧结后的无机粘结剂/TiC复合材料的钛元素XPS分析,图谱在454.3eV处存在一个微弱的小峰,这对应于Ti-O-Fe键,说明在烧结过程中TiC能与无机粘接剂形成Ti-O-Fe键,这有利于提高粘接剂对TiC粉末的粘接强度。
(2)无机粘结剂/TiC复合材料成型料的配制
无机粘结剂/TiC复合材料成型料的重量百分比配方如下:
TiC粉末(直径1-10微米) 70%-80%
无机粘结剂 15%-27%
无水乙醇 3%-5%
成型料中无水乙醇的加入,在混料时会在TiC和无机粘结剂粉末表面形成一层无水乙醇液膜,使粉末之间产生一定的毛细管力,防止TiC和无机粘结剂粉末在混料过程中因为密度差异而产生分层,便于TiC和无机粘结剂粉末混合均匀。
(3)无机粘结剂/TiC复合材料的烧结
将无机粘结剂/TiC复合材料成型料称取相应重量后倒入石墨模具中,放入热压炉中,在氩气保护气氛下,以5-8℃/min的速度升温至900-950℃,在该温度下无机粘结剂软化成粘流态,在20-40MPa成型压力作用下,无机粘结剂填充到TiC粉末的间隙中。在烧结温度下保温30-50min,保温过程中无机粘结剂进一步润湿TiC粉末,并与TiC粉末表面产生化学键合。保温完成后模具带压随炉冷却,当温度低于700℃时,无机粘结剂凝固成固态,与TiC粉末形成牢固的粘接体,此时可卸除压力同时停止输送氩气,模具继续随炉冷却,当炉温冷却到70℃以下时,开炉打开模具,获得无机粘结剂/TiC复合材料零件成品。
先采用熔炼法制备出与TiC粉末粘接性良好的TiC材料专用的无机粘接剂,再将无机粘接剂粉末与TiC粉末混合均匀后热压烧结,制备出一种无机粘结剂/TiC复合材料
本发明的有益效果:
本发明通过该方法能制备出显微结构均匀致密的无机粘结剂/TiC复合材料(参见图3),热压烧结后无机粘接剂与TiC粉末界面结合良好(参见图4),材料抗弯强度能达到200MPa,硬度达到HRC54-62,在5wt%的盐酸溶液中浸泡24h,材料表面无明显的腐蚀现象,与普通的TM52TiC钢结合金相比具有良好的耐酸性能(参见图5、图6),该材料可以在某些酸性环境下作为耐磨材料使用。
附图说明
图1原料TiC粉末的钛元素XPS分析。
图2烧结后的无机粘结剂/TiC复合材料的钛元素XPS分析。
图3烧结后的无机粘结剂/TiC复合材料的断口显微形貌。
图4烧结后的无机粘结剂/TiC复合材料中的TiC与无机粘结剂的界面形貌。
图5无机粘结剂/TiC复合材料在5wt%的盐酸溶液中浸泡24h后的表面形貌。
图6 TM52TiC钢结合金在5wt%的盐酸溶液中浸泡10min后的表面形貌。
具体实施方式
参见附图。
下面结合实施例对本发明作进一步说明。
实施例
本实施例提供一种无机粘结剂以及无机粘结剂/TiC复合材料的制备方法具体步骤为:
(1)采用高温熔炼法制备无机粘接剂:
(a) 一种无机粘结剂,各原料组分的重量百分比为:
硼酸 8%
氧化铋 15%
碳酸钾 5%%
氧化锆 4%
三氧化二铬 3%
三氧化二铁 4%
二氧化硅 61%
一种无机粘结剂/TiC复合材料的制备方法具体步骤为:
(1)采用高温熔炼法制备无机粘接剂:
(a)将称好的各种原料倒入行星式球磨机的刚玉球磨坛中,刚玉球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球磨球占50% ,直径小于10mm的刚玉球磨球占50%。刚玉球磨坛自转速度为400r/min,公转速度为120 r/min。原料球磨混合60min后取出,获得无机粘结剂的熔炼原料料粉。
(b)无机粘结剂的熔炼与破碎
将坩埚炉以5℃/min的速度,升温到1450℃,塞上堵料杆,倒入混好的料粉,倒入熔炼原料料粉的体积为坩埚体积的1/2,在坩埚炉出料口处放一装满水的不锈钢容器。待炉温再次升到1450℃时,保温1.5h,提起堵料杆让熔化的无机粘结剂的熔炼原料流入水中进行水淬,得到无机粘结剂碎块。
将水淬后的无机粘结剂碎块收集,倒入行星式球磨机的刚玉球磨坛中,加入与无机粘结剂碎块等重的水,球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为20mm的刚玉球磨球占30% ,直径10-20mm的刚玉球磨球占70%。刚玉球磨坛自转速度为800r/min,公转速度为150 r/min,无机粘结剂碎块球磨8h后,得到无机粘结剂浆料,将得到的无机粘结剂浆料倒入盛料盘中。
(c) 无机粘结剂的干燥过筛
将无机粘结剂浆料在120℃下干燥,待无机粘结剂浆料完全干透后用塑料铲将其铲起再倒入行星式球磨机的刚玉球磨坛中,球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球磨球占50% ,直径小于10mm的刚玉球磨球占50%。刚玉球磨坛自转速度为400r/min,公转速度为120 r/min,原料球磨2h后将粉体倒出过400#筛,过筛后得到无机粘结剂,将无机粘结剂封袋后放在干燥塔中,待用;
(2)无机粘结剂/TiC复合材料成型料的配制
无机粘结剂/TiC复合材料成型料的重量百分比配方如下:
TiC粉末(直径1-10微米) 75%
无机粘结剂 20%
无水乙醇 5%
将称好的各种原料组分倒入行星式球磨机的刚玉球磨坛中,球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球磨球占50% ,直径小于10mm的刚玉球磨球占50%。刚玉球磨坛自转速度为400r/min,公转速度为120 r/min。原料球磨混合60min后取出,获得无机粘结剂/TiC复合材料成型料。
(3)无机粘结剂/TiC复合材料的烧结
根据零件尺寸称取相应重量的无机粘结剂/TiC复合材料成型料后,倒入石墨模具中,并将该石墨模具组装好后,放入热压炉中,在氩气保护气氛下,以8℃/min的速度升温至950℃,保温40min,保温同时施加40MPa的成型压力,保温完成后石墨模具带压随炉冷却,当温度低于700℃时,卸除压力同时停止输送氩气,模具继续随炉冷却,当炉温冷却到60℃时,开炉打开石墨模具,获得无机粘结剂/TiC复合材料零件成品。
Claims (3)
1.一种无机粘结剂,其特征在于:其各原料组分的重量百分比配方如下:
硼酸 5%-8%
氧化铋 10%-15%
碳酸钾 5%-8%
氧化锆 3%-4%
三氧化二铬 3%-4%
三氧化二铁 2%-4%
二氧化硅 57%-72%。
2.根据权利要求其所述的一种无机粘结剂/TiC复合材料的制备方法,其特征在于:依次包括以下步骤:
(1)采用高温熔炼法制备无机粘接剂:
(a) 将称好的各种原料组分倒入行星式球磨机的刚玉球磨坛中,刚玉球磨坛直径150mm,按球料质量比1-1.4:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球磨球占50%,直径小于10mm的刚玉球磨球占50%。刚玉球磨坛自转速度为350-450r/min,公转速度为100-140 r/min。原料球磨混合30-60min后取出,获得无机粘结剂的熔炼原料料粉;
(b)无机粘结剂的熔炼与破碎
将坩埚炉以2-5℃/min的速度,升温到1430-1450℃,塞上堵料杆,倒入混好的熔炼原料料粉,倒入熔炼原料料粉的体积为坩埚体积的1/2-2/3,在坩埚炉出料口处放一装满水的不锈钢容器;待炉温再次升到1430-1450℃时,保温1-2h,提起堵料杆让熔化的熔炼原料料粉流入水中进行水淬,得到无机粘结剂碎块;
将水淬后的无机粘结剂碎块收集,倒入行星式球磨机的刚玉球磨坛中,加入与无机粘结剂碎块等重的水,球磨坛直径150mm,按球料质量比1-1.4:1的比例加入刚玉球磨球,其中直径为20mm的刚玉球占30% ,直径为10-20mm的刚玉球占70%;球磨坛自转速度为600-800r/min,公转速度为120-150 r/min,无机粘结剂碎块球磨8-12h后得到无机粘结剂浆料,将得到的无机粘结剂浆料倒入盛料盘中;
(c) 无机粘结剂的干燥过筛
将无机粘结剂浆料在110-130℃下干燥,待无机粘结剂浆料完全干透后用塑料铲将其铲起倒入行星式球磨机的刚玉球磨坛中,刚玉球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球磨球占50% ,直径小于10mm的刚玉球磨球占50%;刚玉球磨坛自转速度为400r/min,公转速度为120 r/min,原料球磨2-4h后得到无机粘结剂粉体,将无机粘结剂粉体倒出过350-450#筛,过筛后得到无机粘结剂,将无机粘结剂封袋后放在干燥塔中,待用;
(2)无机粘结剂/TiC复合材料成型料的配制
无机粘结剂/TiC复合材料的各原料组分的重量百分比配方如下:
TiC粉末(直径1-10微米) 70%-80%
无机粘结剂 15%-27%
无水乙醇 3%-5%
将称好的各种原料组分倒入行星式球磨机的刚玉球磨坛中,刚玉球磨坛直径150mm,按球料质量比1-1.4:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球占50% ,直径小于10mm的刚玉球占50%;刚玉球磨坛自转速度为350-450r/min,公转速度为100-140 r/min;原料球磨混合30-60min后取出,获得无机粘结剂/TiC复合材料成型料;
(3)无机粘结剂/TiC复合材料的烧结
根据零件尺寸称取相应重量的无机粘结剂/TiC复合材料成型料,再倒入石墨模具中,并将该石墨模具组装好后,放入热压炉中,在氩气保护气氛下,以5-8℃/min的速度升温至900-950℃,保温30-50min,保温同时施加20-40MPa的成型压力,保温完成后石墨模具带压随炉冷却,当温度低于700℃时,卸除压力同时停止输送氩气,石墨模具继续随炉冷却,当炉温冷却到70℃以下时,开炉打开模具,获得无机粘结剂/TiC复合材料零件成品。
3.根据权利要求1所述的一种无机粘结剂/TiC复合材料的制备方法,其特征在于,依次包括以下步骤:
(1)采用高温熔炼法制备无机粘接剂:
(a) 将称好的各种原料组分倒入行星式球磨机的刚玉球磨坛中,刚玉球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球磨球占50% ,直径小于10mm的刚玉球磨球占50%。刚玉球磨坛自转速度为400r/min,公转速度为120 r/min。原料球磨混合30-60min后取出,获得无机粘结剂的熔炼原料料粉;
(b)无机粘结剂的熔炼与破碎
将坩埚炉以2-5℃/min的速度,升温到1430-1450℃,塞上堵料杆,倒入混好的熔炼原料料粉,倒入熔炼原料料粉的体积为坩埚体积的1/2-2/3,在坩埚炉出料口处放一装满水的不锈钢容器;待炉温再次升到1430-1450℃时,保温1-2h,提起堵料杆让熔化的熔炼原料料粉流入水中进行水淬,得到无机粘结剂碎块;
将水淬后的无机粘结剂碎块收集,倒入行星式球磨机的刚玉球磨坛中,加入与无机粘结剂碎块等重的水,球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为20mm的刚玉球占30% ,直径为10-20mm的刚玉球占70%;球磨坛自转速度为600-800r/min,公转速度为120-150 r/min,无机粘结剂碎块球磨8-12h后得到无机粘结剂浆料,将得到的无机粘结剂浆料倒入盛料盘中;
(c) 无机粘结剂的干燥过筛
将无机粘结剂浆料在120℃下干燥,待无机粘结剂浆料完全干透后用塑料铲将其铲起倒入行星式球磨机的刚玉球磨坛中,刚玉球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球磨球占50% ,直径小于10mm的刚玉球磨球占50%;刚玉球磨坛自转速度为400r/min,公转速度为120 r/min,原料球磨2-4h后得到无机粘结剂粉体,将无机粘结剂粉体倒出过400#筛,过筛后得到无机粘结剂,将无机粘结剂封袋后放在干燥塔中,待用;
(2)无机粘结剂/TiC复合材料成型料的配制
无机粘结剂/TiC复合材料的各原料组分的重量百分比配方如下:
TiC粉末(直径1-10微米) 70%-80%
无机粘结剂 15%-27%
无水乙醇 3%-5%
将称好的各种原料组分倒入行星式球磨机的刚玉球磨坛中,刚玉球磨坛直径150mm,按球料质量比1.2:1的比例加入刚玉球磨球,其中直径为10mm的刚玉球占50% ,直径小于10mm的刚玉球占50%;刚玉球磨坛自转速度为400r/min,公转速度为120 r/min;原料球磨混合30-60min后取出,获得无机粘结剂/TiC复合材料成型料;
(3)无机粘结剂/TiC复合材料的烧结
根据零件尺寸称取相应重量的无机粘结剂/TiC复合材料成型料,再倒入石墨模具中,并将该石墨模具组装好后,放入热压炉中,在氩气保护气氛下,以5-8℃/min的速度升温至900-950℃,保温30-50min,保温同时施加20-40MPa的成型压力,保温完成后石墨模具带压随炉冷却,当温度低于700℃时,卸除压力同时停止输送氩气,石墨模具继续随炉冷却,当炉温冷却到70℃以下时,开炉打开模具,获得无机粘结剂/TiC复合材料零件成品。
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