CN105884375A - Liquid phase sintering method of Si3N4-TiZrN2-TiN composite conductive ceramic - Google Patents

Liquid phase sintering method of Si3N4-TiZrN2-TiN composite conductive ceramic Download PDF

Info

Publication number
CN105884375A
CN105884375A CN 201610178439 CN201610178439A CN105884375A CN 105884375 A CN105884375 A CN 105884375A CN 201610178439 CN201610178439 CN 201610178439 CN 201610178439 A CN201610178439 A CN 201610178439A CN 105884375 A CN105884375 A CN 105884375A
Authority
CN
Grant status
Application
Patent type
Prior art keywords
si3n4
tin
conductive ceramic
tizrn2
composite conductive
Prior art date
Application number
CN 201610178439
Other languages
Chinese (zh)
Other versions
CN105884375B (en )
Inventor
江涌
吴澜尔
黄新华
Original Assignee
北方民族大学
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • C04B35/587Fine ceramics
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225Yttrium oxide or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3227Lanthanum oxide or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38Non-oxide ceramic constituents or additives
    • C04B2235/3852Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
    • C04B2235/3865Aluminium nitrides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38Non-oxide ceramic constituents or additives
    • C04B2235/3852Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
    • C04B2235/3886Refractory metal nitrides, e.g. vanadium nitride, tungsten nitride
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54Particle size related information
    • C04B2235/5418Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54Particle size related information
    • C04B2235/5418Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5454Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658Atmosphere during thermal treatment

Abstract

Provided is Si3N4-TiZrN2-TiN composite conductive ceramic. Raw materials for synthesizing the composite conductive ceramic comprise Si3N4, ZrN, TiN, Y2O3, La2O3 and AlN. The final product of the composite conductive ceramic comprises an Si3N4 phase, a TiN phase and a solid solution TiZrN2 phase of metal nitride. Due to addition of AlN, volatilization caused by adding of Al2O3 in a conventional mode is avoided, and the surface of the final product to which AlN is added can be smoother than that of the product to which Al2O3 is added. The invention further provides a liquid phase sintering method of the Si3N4-TiZrN2-TiN composite conductive ceramic. The Si3N4-TiZrN2-TiN composite conductive ceramic has the advantages that electrical resistance is low, wherein the sample resistance tested by an SX1944 four-probe tester for the composite conductive ceramic is at the 10-2 omega.cm order which is far lower than that of like products; the mechanical strength is high, wherein the load of the composite conductive ceramic is 10 kg, the pressurizing time is 5 s, the measured Vickers hardness of the sample is 14.7 GPa, the sample breaking tenacity calculated through the hardness indentation quadrangle expansion crack length is 7.8 MPa.m 0.5, and the original strength and hardness of silicon nitride ceramic are kept.

Description

一种S i 3N4-T i ZrN2-T i N复合导电陶瓷的液相烧结法 One kind of S i 3N4-T i ZrN2-T i N composite conductive ceramic phase sintering method

技术领域 FIELD

: :

[0001]本发明涉及导电陶瓷技术领域,具体地说,涉及一种Si3N4-TiZrN2-TiN复合导电陶瓷的液相烧结法。 [0001] The present invention relates to a conductive ceramic technical field, and more particularly, to a liquid-phase Si3N4-TiZrN2-TiN composite conductive ceramic sintering method.

背景技术 Background technique

: :

[0002]氮化硅(Si3N4)是一种性能很好的结构陶瓷材料,具有质量轻、高强度、高硬度、高耐腐蚀性等,可应用于各行各业。 [0002] The silicon nitride (Si3N4) is a good one property structural ceramic material having a light weight, high strength, high hardness, high corrosion resistance, can be used in various industries. 制备氮化硅陶瓷材料的方法很多,有热压、常压、反应等烧结方法,其中常压烧结方法简单易行,耗能少。 Many methods for preparing a silicon nitride ceramic material, sintered hot pressing, pressure, reaction or the like, wherein the atmospheric sintering method is simple, low energy consumption. 由于氮化硅是共价键化合物,自扩散系数低,本身很难直接烧结成瓷,因此往往加入一些氧化物等作为烧结助剂进行烧结。 Since the silicon nitride is a covalent bond compound, low self-diffusion coefficient, directly sintered into the ceramic itself is difficult, and therefore tend to add some other oxide as a sintering aid for sintering. 常用的有Al2O3、Y2O3、Mg02等。 Commonly used Al2O3, Y2O3, Mg02 and so on. 这些添加物在烧结过程中形成液相促使氮化硅陶瓷烧结致密,以达到材料高强度、高硬度的要求。 These additives promote the formation of a liquid phase silicon nitride ceramic sintered compact, to achieve the required high strength materials, high hardness during sintering.

[0003]由于Si3N4陶瓷本身高强度和高硬度的性能使得后期加工困难,常以金刚石刀具进行切割,但传统的金刚石加工的方法加工效率低且成本昂贵。 [0003] Due to the high strength and high hardness of Si3N4 ceramic itself is difficult so that the post-processing, often diamond tool for cutting, but the conventional method of a low processing efficiency of diamond machining and costly. 成本低、效率高的放电(电火花)加工技术已成功用于金属制品加工,若能用于加工Si3N4陶瓷则会大大提高加工效率和降低加工成本,但能用放电加工的材料必须具有一定的导电性,其电阻率要求低达1t3Q.cm量级及以下,但Si3N4陶瓷属于绝缘体,其电阻率约为115 Ω.cm量级,是不可能用放电方法进行加工的。 Low cost and high discharge efficiency (EDM) process technology has been successfully used for processing metal products, if used in the manufacture of Si3N4 would greatly improve the processing efficiency and reduce processing costs, but the material can discharge machining must have a certain conductivity, low resistivity claim 1t3Q.cm magnitude and below, but belongs Si3N4 ceramic insulator, a resistivity of the order of about 115 Ω.cm, it is impossible to perform electrical discharge machining method. 所以人们想到了用另外一种导电性很好的材料加入Si3N4中制备成Si3N4基复合导电性材料,使其电阻率下降到能用于电火花加工的程度。 Add people think so based composite Si3N4 Si3N4 conductive material prepared as in the well with another conductive material, so that resistivity decreases to a level that can be used electro-discharge machining. 在CN1272283C的专利里使用了金属Ti和Ta,从而使最终烧结的复合氮化硅电阻率降到1t3Q.cm量级,刚刚达到放电加工的要求,并且其硬度和断裂韧性较未加导电助剂的氮化硅陶瓷差。 In patent CN1272283C Lane Ti, and Ta, so that the resistivity of the silicon nitride composite sintered reduced 1t3Q.cm final magnitude, just to meet the requirements for electrical discharge machining, and its hardness and fracture toughness than the conductive additive is not added silicon nitride ceramic difference.

发明内容 SUMMARY

: :

[0004]本发明旨在解决上述问题,提供一种电阻率低、硬度和断裂韧性优良的一种Si3N4-TiZrN2-TiN复合导电陶瓷;同时还提供一种Si3N4-TiZrN2-TiN复合导电陶瓷的液相烧结法。 [0004] The present invention is intended to solve the above problems, to provide a low resistivity, excellent hardness and fracture toughness one kind of Si3N4-TiZrN2-TiN composite electrically conductive ceramic; also provides liquid for the Si3N4 TiZrN2 TiN--conductive composite ceramics phase sintering method.

[0005] —种Si3N4-TiZrN2-TiN复合导电陶瓷,合成该复合导电陶瓷的原料包括:Si3N4、ZrN、TiN、Y203、La203、AlN;该复合导电陶瓷的的最终产物里包括Si3N4相、TiN相和金属氮化物的固溶体TiZrN2相。 [0005] - species Si3N4-TiZrN2-TiN composite conductive ceramic, the synthesis of the composite conductive ceramic materials include: Si3N4, ZrN, TiN, Y203, La203, AlN; final product of the composite conductive ceramic's include Si3N4 phase, TiN phase and a solid solution of a metal nitride TiZrN2 phase. 其中,AlN的加入可避免常规方式中加入Al2O3所引起的低温挥发,并且加入AlN会使最终产品的表面比加入Al2O3光滑。 Wherein, the addition of AlN can be avoided in a conventional manner caused by a low-temperature volatilization Al2O3, AlN and makes the final product was added surface smoother than Al2O3 added.

[0006]由于是采用烧结工艺来制作的复合导电陶瓷材料,各材料烧结过程中的热膨胀系数是至关重要的的,如果热膨胀系数相差大,则不利于烧结,会影响最终成品的密度、硬度和断裂韧性,故所选择的导电助剂的除了要电阻率低,还要热膨胀系数要与氮化硅相差不大。 [0006] Since the sintering process is employed to produce the composite conductive ceramic material, the thermal expansion coefficient of each material in the sintering process is critical, and if a large difference in thermal expansion coefficient, is not conducive to the sintering, will affect the density of the final product, the hardness and fracture toughness, it is selected as a conductive additive in addition to a low resistivity, but also to be little difference between the thermal expansion coefficient of silicon nitride. 另外,如果还兼有其它好的机械性能则更为理想。 Further, if it is both good mechanical properties are further more preferable. 氮化钛和氮化锆都有高电导率,两者的电阻率都在10—4Ω.cm量级,ZrN比TiN更低(TiN:2.07X10—4Ω.cm;ZrN:1.4Χ 10—4Ω.cm);热膨胀系数和氮化硅在一个数量级,均为约KT6IT1,且ZrN更接近氮化硅(Si3N4:3.64 XΙΟ-Ι-1;ZrN: 7.3 X KT6IT1;TiN: 9.35 X KT6IT1);另外TiN、ZrN本身都的硬度都比氮化硅高很多,其中,ZrN的硬度比TiN碳化钛更高,ZrN作为添加剂有增强韧性的作用。 Titanium nitride and zirconium nitride have high conductivity, resistivity both in the order of 10-4Ω.cm, ZrN lower than TiN (TiN: 2.07X10-4Ω.cm; ZrN: 1.4Χ 10-4Ω .cm); and coefficient of thermal expansion of silicon nitride in an order of magnitude, are approximate KT6IT1, ZrN and closer to the silicon nitride (Si3N4: 3.64 XΙΟ-Ι-1; ZrN: 7.3 X KT6IT1; TiN: 9.35 X KT6IT1); additionally TiN, ZrN itself is much higher hardness than silicon nitride, wherein, ZrN higher hardness than titanium carbide TiN, ZrN role as an additive to enhance the toughness.

[0007]优选的,Si3N4:TiN: Y2O3: La2O3: AlN= (9〜11): (5.4〜6.6): (0.8〜1.2): (0.8〜1.2):(1.3〜1.66),2洲的加入量为8〜15¥戈%。 [0007] preferably, Si3N4: TiN: Y2O3: La2O3: AlN = (9~11): (5.4~6.6): (0.8~1.2): (0.8~1.2) :( 1.3~1.66), 2 Chau added the amount of 8~15 ¥ ge%.

[0008] 一种S i 3N4-T i ZrN2-T iN复合导电陶瓷的液相烧结法,包括以下步骤: [0008] A S i 3N4-T i ZrN2-T iN composite conductive ceramic phase sintering method, comprising the steps of:

[0009] (1)配料混合:将513〜、1^1丫203、1^203、八1~以(9〜11):(5.4〜6.6):(0.8〜1.2):(0.8〜1.2): (1.3〜1.66)的比例混合,ZrN的加入量为8〜15w.t %,之后在研钵中加入酒精研磨I〜3h后干燥;其中,Si3N4的α相含量高于70%,纯度高于97%,粒度为0.6〜0.8μπι,TiN粒度为18〜22nm,ZrN粒度为16〜21nm; [0009] (1) mixing the ingredients: The 513~, 203,1 ^ 1 ^ 1 203 Ah, 1 ~ to eight (9~11) :( 5.4~6.6) :( 0.8~1.2) :( 0.8~1.2) : (1.3~1.66) mixing ratio, the amount of ZrN was added 8~15w.t%, after the addition of alcohol after drying I~3h milling in a mortar; wherein, [alpha] Si3N4 phase content is higher than 70%, high purity 97% particle size of 0.6~0.8μπι, TiN particle size of 18~22nm, ZrN particle size of 16~21nm;

[0010] (2)成型及烧结:将干燥后的混合料用模具干压成型再经冷等静压后放入烧结炉中在N2保护气氛中进行烧结,烧结温度为1760±25°C,保温时间根据样品的大小可设为I〜3h。 [0010] (2) molding and sintering: the dried mixture by dry pressing mold after cold isostatic pressing and then put into a furnace in an N2 atmosphere for sintering, the sintering temperature is 1760 ± 25 ° C, the size of the sample holding time may be set I~3h.

[0011]本发明有益效果如下: [0011] Advantageous effects of the present invention are as follows:

[0012] 1.电阻率低;本发明的复合导电陶瓷用SX1944四探针测试仪测试样品电阻为10—2Ω.cm量级,远低于同类产品。 [0012] 1. low resistivity; electrically conductive ceramic composite of the present invention SX1944 four-probe resistance tester sample 10-2Ω.cm magnitude, much lower than similar products.

[0013] 2.机械强度高;本发明的复合导电陶瓷用载荷为10kg,加压时间为5s的条件测量样品的维氏硬度为14.7GPa;利用硬度压痕四角处扩展的裂纹长度计算样品的断裂韧性为7.SMPa.n/3.5,达到了氮化硅陶瓷原有的高硬度和高断裂韧性。 [0013] 2. High mechanical strength; electrically conductive ceramic composite of the present invention is a load of 10kg, pressing time 5s condition of the sample is measured Vickers hardness 14.7GPa; indentation hardness using four corners of the extended sample is calculated crack length fracture toughness 7.SMPa.n / 3.5, to achieve the original silicon nitride ceramic high hardness and fracture toughness.

具体实施方式 detailed description

: :

[0014] 一种Si3N4-TiZrN2-TiN复合导电陶瓷,合成该复合导电陶瓷的原料包括:Si3N4、ZrN、TiN、Y203、La203、AlN;该复合导电陶瓷的的最终产物里包括Si3N4相、TiN相和金属氮化物的固溶体Ti ZrN2相。 [0014] A Si3N4-TiZrN2-TiN composite conductive ceramic, synthetic material of the composite conductive ceramic comprises: Si3N4, ZrN, TiN, Y203, La203, AlN; the final product in a composite conductive ceramic phase comprises Si3N4, TiN phase and a solid solution of a metal nitride with Ti ZrN2.

[0015]在本实施方式中,513他:!1化¥203:1^203:厶^=(9〜11):(5.4〜6.6):(0.8〜1.2):(0.8〜1.2):(1.3〜1.66),2洲的加入量为8〜15界.七%。 [0015] In the present embodiment, he 513:! 1 of ¥ 203: 1 ^ 203: ^ Si = (9~11) :( 5.4~6.6) :( 0.8~1.2) :( 0.8~1.2) :( 1.3~1.66), addition of 2 continents is 8~15 community. seven percent.

[0016] 一种Si3N4-TiZrN2-TiN复合导电陶瓷的液相烧结法,Si3N4选用α相含量高于70%粉料,纯度高于97%,平均粒度0.7μπι; Y2O3、La2O3和AlN为市售,化学纯;TiN购自合肥凯尔纳米能源科技股份有限公司,纯度为99.2%,平均粒度为20nm;ZrN购自锦州金鑫股份有限公司;将各成分按(9〜11):():(5.4〜6.6):(0.8〜1.2):(0.8〜1.2):(1.3〜1.66)的比例称量配料,将配好的料加入酒精在玛瑙研钵中混磨2小时或加入酒精和ZrO2球在聚氨酯筒中球磨I小时后置于空气中干燥;再将干燥好的混合料用不锈钢磨具干压成方块后放入烧结炉中在N2保护气氛中进行烧结,烧结温度为1760°C±25°C,保温时间根据样品的大小可设为l_3h。 [0016] A liquid Si3N4-TiZrN2-TiN composite conductive ceramic sintering method, Si3N4 selection α content greater than 70% relative to the powder, purity of more than 97%, an average particle size 0.7μπι; Y2O3, La2O3, and are commercially available AlN , chemically pure; available from Hefei Kyle nanometers of TiN eNERGY CORP., purity 99.2%, average particle size of 20nm; ZrN available from Jinzhou Co. jinxin; by each component (9~11) :() :( 5.4~6.6) :( 0.8~1.2) :( 0.8~1.2) :( 1.3~1.66) ratio of the ingredients were weighed, ethanol was added with a good feed mill mixed in an agate mortar for two hours or ZrO2 ball added alcohol and in the polyurethane cylinder I after milling was dried in air hours; then the dried mixture into a stainless steel abrasive sintered in a sintering furnace in an atmosphere of dry N2 protection pressed into a block, the sintering temperature is 1760 ° C ± 25 ° C, the holding time can be set according to the size of the sample l_3h.

[0017]利用日本理学D/MAX-RB型X射线衍射仪对烧结进行样品的物相分析,证实样品内含有金属氮化物的固溶体TiZrN2。 [0017] using a Rigaku D / MAX-RB X-ray diffraction of the sintered samples was performed phase analysis confirmed the solid solution containing the sample TiZrN2 metal nitride.

Claims (3)

  1. 1.一种Si3N4-TiZrN2-TiN复合导电陶瓷,其特征在于:合成该复合导电陶瓷的原料包括:Si3N4、ZrN、TiN、Y203、La203、AlN;该复合导电陶瓷的的最终产物里包括Si3N4相、TiN相和金属氮化物的固溶体TiZrfe相。 An Si3N4 TiN-TiZrN2-electrically conductive ceramic composite, which is characterized in that: the synthetic material of the composite conductive ceramic comprises: Si3N4, ZrN, TiN, Y203, La203, AlN; the final product in a composite conductive ceramic phase comprises Si3N4 , TiN phase and a solid solution phase of metal nitride TiZrfe.
  2. 2.如权利要求1所述的一种Si3N4-TiZrN2-TiN复合导电陶瓷,其特征在于:Si3N4:TiN:Y203:La203:AlN=(9〜ll):(5.4〜6.6):(0.8〜1.2):(0.8〜1.2):(1.3〜1.66),Zrr^]WA量为8〜15w.t%。 2. An claim 1 Si3N4-TiZrN2-TiN composite conductive ceramic claim, wherein: Si3N4: TiN: Y203: La203: AlN = (9~ll) :( 5.4~6.6) :( 0.8~1.2 ) :( 0.8~1.2) :( 1.3~1.66), Zrr ^] WA amount 8~15w.t%.
  3. 3.一种Si3N4-TiZrN2-TiN复合导电陶瓷的液相烧结法,其特征在于:包括以下步骤: (1)配料混合:将313〜、1^1丫203、1^203、八1~以(9〜11):(5.4〜6.6):(0.8〜1.2):(0.8〜1.2): (1.3〜1.66)的比例混合,ZrN的加入量为8〜15w.t%,之后在研钵中加入酒精研磨I〜3h后干燥;其中,Si3N4的α相含量高于70%,纯度高于97%,粒度为0.6〜0.8μπι,TiN粒度为18〜22nm,ZrN粒度为16〜21nm; (2)成型及烧结:将干燥后的混合料用模具干压成型再经冷等静压后放入烧结炉中在N2保护气氛中进行烧结,烧结温度为1760 ± 25 °C,保温时间为I〜3h。 A Si3N4 TiZrN2 TiN--electrically conductive ceramic composite liquid phase sintering method, characterized by: comprising the steps of: (1) mixing the ingredients: The 313~, 203,1 ^ 1 ^ 1 203 Ah, eight to 1 (9~11) :( 5.4~6.6) :( 0.8~1.2) :( 0.8~1.2): (1.3~1.66) mixing ratio, the amount of ZrN was added 8~15w.t%, after the mortar dried after alcohol grinding I~3h; wherein, [alpha] Si3N4 phase content is higher than 70% purity of more than 97%, a particle size of 0.6~0.8μπι, TiN particle size of 18~22nm, ZrN particle size of 16~21nm; (2 ) molding and sintering: the mix dry mold press forming after drying after cold isostatic pressing and then put into a furnace in a N2 atmosphere sintering, the sintering temperature is 1760 ± 25 ° C, holding time I~ 3h.
CN 201610178439 2016-03-18 2016-03-18 Species SiN-TiZrN-TiN composite conductive ceramic phase sintering method CN105884375B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201610178439 CN105884375B (en) 2016-03-18 2016-03-18 Species SiN-TiZrN-TiN composite conductive ceramic phase sintering method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201610178439 CN105884375B (en) 2016-03-18 2016-03-18 Species SiN-TiZrN-TiN composite conductive ceramic phase sintering method

Publications (2)

Publication Number Publication Date
CN105884375A true true CN105884375A (en) 2016-08-24
CN105884375B CN105884375B (en) 2018-05-22

Family

ID=57014909

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201610178439 CN105884375B (en) 2016-03-18 2016-03-18 Species SiN-TiZrN-TiN composite conductive ceramic phase sintering method

Country Status (1)

Country Link
CN (1) CN105884375B (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100009839A1 (en) * 2006-06-09 2010-01-14 Antionette Can Ultrahard Composite Materials
CN102170716A (en) * 2010-12-09 2011-08-31 江苏华盛精细陶瓷科技有限公司 Method for manufacturing silicon nitride heating body
CN103096528A (en) * 2010-12-09 2013-05-08 江苏华盛精细陶瓷科技有限公司 Preparation method for silicon nitride heating body
CN103764595A (en) * 2011-06-21 2014-04-30 戴蒙得创新股份有限公司 Composite compacts formed of ceramics and low-volume cubic boron nitride and method of manufacture

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100009839A1 (en) * 2006-06-09 2010-01-14 Antionette Can Ultrahard Composite Materials
CN102170716A (en) * 2010-12-09 2011-08-31 江苏华盛精细陶瓷科技有限公司 Method for manufacturing silicon nitride heating body
CN103096528A (en) * 2010-12-09 2013-05-08 江苏华盛精细陶瓷科技有限公司 Preparation method for silicon nitride heating body
CN103764595A (en) * 2011-06-21 2014-04-30 戴蒙得创新股份有限公司 Composite compacts formed of ceramics and low-volume cubic boron nitride and method of manufacture

Also Published As

Publication number Publication date Type
CN105884375B (en) 2018-05-22 grant

Similar Documents

Publication Publication Date Title
Mutsuddy et al. Ceramic injection molding
Wang et al. Influence of hot pressing sintering temperature and time on microstructure and mechanical properties of TiB2 ceramics
Watanahe et al. Mechanical Properties of Hot‐Pressed TiB2‐ZrO2 Composites
Tsukama et al. Thermal stability of Y 2 O 3-partially stabilized zirconia (Y-PSZ) and Y-PSZ/Al 2 O 3 composites
Guo et al. Mechanical behavior of two-step hot-pressed ZrB2-based composites with ZrSi2
CN101429037A (en) Aluminum-carbon sliding tile and method of producing the same
Zhang et al. Effect of graphite flake on the mechanical properties of hot pressed ZrB2–SiC ceramics
Zhang et al. Microstructure and properties of silicon carbide whisker reinforced zirconium diboride ultra-high temperature ceramics
Li et al. Mechanical properties and electrical conductivity of TiN–Al2O3 nanocomposites
Königshofer et al. Solid-state properties of hot-pressed TiB2 ceramics
Gu et al. Improvements in mechanical properties of TiB2 ceramics tool materials by the dispersion of Al2O3 particles
Becher et al. Temperature‐Dependent Viscosity of SiREAl‐Based Glasses as a Function of N: O and RE: Al Ratios (RE= La, Gd, Y, and Lu)
CN101830717A (en) Zirconium sol reinforced corundum-mullite product and production method thereof
US4769350A (en) Silicon nitride sintered material for cutting tools and process for making the same
Morishima et al. Development of Aluminum Titanate‐Mullite Composite Having High Thermal Shock Resistance
Sheng et al. Preparation of glass-infiltrated 3Y-TZP/Al2O3/glass composites
Luo et al. Effect of composition on properties of alumina/titanium silicon carbide composites
CN101857438A (en) Method for preparing aluminum oxide-titanium carbide-zirconium oxide nanocomposite ceramic material
Fukuhara Properties of (Y) ZrO2–Al2O3 and (Y) ZrO2–Al2O3–(Ti or Si) C Composites
CN1552665A (en) High-performance abrasive ceramic nozzle and producing method thereof
CN1051900A (en) Silicon nitride compound phase ceramic knife tool material with whiskers for supplementing toughness and strength
CN1337377A (en) Intermatallic Ti-Al compound/alumina ceramic composite material and its prepn process
US5302329A (en) Process for producing β-sialon based sintered bodies
CN1533999A (en) Low temperature sintered 99 aluminium oxide ceramic and its production method and use
CN1498876A (en) Method for preparing composite engineering ceramics material of nano ZrO2 (Y2O3)/A12O3/Cu

Legal Events

Date Code Title Description
C06 Publication
C10 Entry into substantive examination
C10 Entry into substantive examination
GR01