CN104418595B - A kind of manufacture method of Sialon ceramics target - Google Patents

A kind of manufacture method of Sialon ceramics target Download PDF

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Publication number
CN104418595B
CN104418595B CN201310370661.9A CN201310370661A CN104418595B CN 104418595 B CN104418595 B CN 104418595B CN 201310370661 A CN201310370661 A CN 201310370661A CN 104418595 B CN104418595 B CN 104418595B
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sialon ceramics
sialon
manufacture method
target
ceramics target
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CN104418595A (en
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姚力军
相原俊夫
大岩彦
大岩一彦
潘杰
王学泽
王科
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Ningbo Jiangfeng hot isostatic pressing technology Co.,Ltd.
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Ningbo Jiangfeng Electronic Material Co Ltd
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Abstract

The invention provides the manufacture method of a kind of Sialon ceramics target.Including: the material powder including silicon nitride, aluminium oxide, aluminium nitride, sintering aid and conductive agent is provided;And by after described material powder mix homogeneously, carry out hot pressed sintering process, form Sialon ceramics target.The Sialon ceramics using the present invention to prepare has good electric conductivity and heat conductivility, thus in filament cutting technique, the spark discharge of pulse feature is constantly produced between wire electrode in strengthening Sialon ceramics and moving, and when spark discharge instantaneous generation high temperature, accelerate the ablation of Sialon ceramics and the contact site of wire electrode, improve the cutting performance of Sialon ceramics, improve the smoothness of cutting Sialon ceramics, and the machining accuracy of Sialon ceramics.

Description

A kind of manufacture method of Sialon ceramics target
Technical field
The present invention relates to quasiconductor sputtering field, particularly to the manufacture method of a kind of Sialon ceramics target.
Background technology
Sai Long (sialon) be a kind of basic structural unit be (Si, Al) (O, N)4Tetrahedron material, It is commonly used in ceramic material.Sialon ceramics includes α-sialon(MeXSi12-(m+n)Alm+n) OnN16-n, Me is metal ion, including yttrium etc.) and β-sialon(Si6-ZAlZOZN8-Z) two kinds of deformable bodys.
Wherein, sialon pottery is silicon nitride (Si3N4) and aluminium oxide (Al2O3) consolidating of at high temperature generating Solution, the characteristic of the crystalline phase that two kinds of sialon potteries inherit silicon nitride and two kinds of materials of aluminium oxide is the highest firmly While degree, wearability, the most each tool characteristic.As α-sialon also has thermal shock resistance, and β-sialon compares In conventional ceramic, there is more preferable fracture toughness.Sialon pottery has good heat, power, optical property, and Stable chemical nature, is important inorganic material.And the complex phase being made up of α-sialon and β-sialon is matched grand Pottery the most also has high intensity and high tenacity concurrently.
Based on the mechanical performance that sialon pottery is good, sialon pottery is usually used in bearing, sealing ring, Yi Jiguang Learn the wear parts in the semiconductor device such as device, quasiconductor deviding device.Wherein, in semiconductor applications, Sialon pottery forms the element such as optics, quasiconductor deviding device by vacuum magnetron sputtering coating film mode Wear parts.More refer to the China of Publication No. CN102307827A specially about sialon pottery introduction Profit document.
In vacuum magnetron sputtering coating film technique, sialon ceramic target is placed on the target chamber of sputtering base station In body, on base material, form one layer of nanoscale or micron-sized sialon ceramic membrane by ion sputtering mode. The accuracy requirement of thickness based on sialon ceramic membrane, vacuum magnetron sputtering coating film technique is used Sialon ceramic target must mate with the target cavity of sputtering machine table completely.
Existing sialon ceramic target processing technology, makes and mechanical process including target, first leads to Cross hot pressing (HP), without techniques such as pressure (PLS), air pressure (GPS) and hot isotatic pressings (HIP) Form target, realize the structure of sialon ceramic target by machining modes such as line cuttings afterwards and accurately add Work, so that the target cavity of used time and sputtering machine table matches.
But, in sialon ceramic target carries out line cutting process, Sialon ceramics target fragmentation usually occurs Situation, and the deviation of the processing of sialon ceramic target is relatively big, machining accuracy is difficult to ensure, causes Sai Longtao The yield rate of porcelain target is low.
Thus, how to improve the cuttability of sialon pottery, be ability to improve sialon pottery cutting accuracy The problem that field technique personnel need solution badly.
Summary of the invention
For solving the problems referred to above, the invention provides the manufacture method of a kind of Sialon ceramics target, use this Invention obtains Sialon ceramics and is prone to machining, thus improves the machining accuracy of Sialon ceramics target.
The manufacture method of a kind of Sialon ceramics target that the present invention provides, including:
The material powder including silicon nitride, aluminium oxide, aluminium nitride, sintering aid and conductive agent is provided;
After described material powder mix homogeneously, carry out hot pressed sintering process, form Sialon ceramics target.
Alternatively, described conductive agent is metal nitride.
Alternatively, described metal nitride is titanium nitride or tantalum nitride.
Alternatively, the weight content of described silicon nitride, aluminium oxide, aluminium nitride, sintering aid and conductive agent For: 45~60wt%, 2~10wt%, 2~5wt%, 5~10wt%, 30~45wt%.
Alternatively, described hot pressed sintering process technique includes:
It is heated to 1200 DEG C with the speed of 5~10 DEG C/min;
Afterwards, it is heated to 1300~1400 DEG C with the speed of 1.5~3 DEG C/min;
Afterwards, it is heated to 1450~1700 DEG C with the speed of 4~6 DEG C/min;
With 0.3~0.5MPa/min speed persistent pressure, to presetting pressure, described default pressure is more than 20MPa;
And be 1450~1700 DEG C in temperature, preset heat-insulation pressure keeping heating 4~7h under pressure conditions.
Alternatively, described default pressure is 20~30MPa.
Alternatively, described hot pressed sintering processes and carries out under protective atmosphere.
Alternatively, described protective atmosphere includes Ar, He or N2Atmosphere.
Alternatively, it is ball-milling technology by the method for material powder mix homogeneously.
Alternatively, described ball-milling technology includes:
Described material powder is placed in ball grinder, after inserting disperse medium, ball milling 16~24h.
Alternatively, described ball-milling technology includes: using zirconium oxide or aluminium oxide as ball-milling medium.
Alternatively, described disperse medium is dehydrated alcohol and/or glycerol.
Alternatively, also include: after described ball-milling technology, described material powder is dried process.
Alternatively, the temperature of described dried is less than the boiling point of disperse medium.
Compared with prior art, technical scheme has the advantage that
In silicon nitride, aluminium oxide, aluminium nitride, sintering aid, add conductive agent, and process through hot pressed sintering The technique preparing Sialon ceramics, can be effectively improved the electric conductivity that Sialon ceramics is overall, and lead at Sialon ceramics After entering electric current, promote the heat conductivility of Sialon ceramics target based on the good electric conductivity that Sialon ceramics is overall. In such as filament cutting technique, during good conduction and heat conductivility are strengthened Sialon ceramics target and are moved The spark discharge of the pulse feature constantly produced between wire electrode, and the instantaneous generation high temperature when spark discharge, Accelerate the ablation of Sialon ceramics target and the contact site of wire electrode, improve the cutting of Sialon ceramics target Can, improve the smoothness of cutting Sialon ceramics target, thus promote the machining accuracy of Sialon ceramics.
Accompanying drawing explanation
Fig. 1 is the flow chart of the manufacture method of Sialon ceramics target of the present invention;
Fig. 2 is during the present invention makes Sialon ceramics target, uses the embodiment of ball-milling technology mixing raw material Schematic diagram;
Fig. 3~Fig. 4 is to use hot pressed sintering to process PROCESS FOR TREATMENT target during the present invention makes Sialon ceramics target The embodiment schematic diagram of material.
Detailed description of the invention
As described in background, in view of the mechanical performance that Sialon ceramics is good, at semiconductor applications, Sialon ceramics thin film, as wear parts, obtains extensively on the elements such as optics, quasiconductor deviding device Application.
But, when Sialon ceramics target carries out line cutting, the defects such as Sialon ceramics target fragmentation usually occur, The cutting accuracy causing Sialon ceramics target is difficult to ensure.Analyze its reason to be attributed to: at Sialon ceramics target In material line cutting process, Sialon ceramics target connects the positive pole of high frequency pulse power supply, wire electrode (such as molybdenum filament) Connect negative pole.After high frequency pulse power supply is energized, need between Sialon ceramics target and the wire electrode moved Produce the spark discharge of pulse feature, and the instantaneous generation high temperature heat source when spark discharge, thus at Sai Longtao On porcelain target, the contact site contacted with wire electrode is by galvano-cautery, it is achieved the cutting of Sialon ceramics target.
But existing Sialon ceramics is dielectric material, its conduction, heat conductivility are poor.During cutting on line, After high frequency pulse power supply energising, electric current cannot be smooth and easy by Sialon ceramics target, thus at Sialon ceramics target The spark discharge of enough pulse features cannot be produced between material and wire electrode, Sialon ceramics target is realized electricity Corrosion, it is achieved Sialon ceramics target cuts smoothly.
To this end, the invention provides the manufacture method of a kind of Sialon ceramics target, it is thus achieved that have good conductive With the Sialon ceramics target of heat conductivity, improve cutting smooth degree and the cutting processing precision of Sialon ceramics target.
Below in conjunction with the accompanying drawings, by specific embodiment, technical scheme is carried out clear, complete Description.
First, with reference to shown in Fig. 1, perform step S1: provide include silicon nitride, aluminium oxide, aluminium nitride, Sintering aid and the material powder of conductive agent.Above-mentioned raw materials powder is used for making Sialon ceramics target.
In subsequent fabrication process, silicon nitride and aluminium oxide reaction make Sialon ceramics.Wherein, as made During β-sialon, Z Si-N in silicon nitride is replaced by Z Al-O;When making α-sialon, nitrogen N Si-N in SiClx is replaced by n Al-O, and m Si-N is replaced by m Al-N, and rear one The electricity price that individual replacement causes is uneven to be compensated by x metal ions M e.The final Sialon ceramics obtained is concrete Structure determine according to different material fiting ratio example.And the complex phase being made up of α-sialon and β-sialon According to material rate, there is above-mentioned reaction in Sialon ceramics simultaneously.
Described sintering aid is chosen as La2O3、Y2O3And Al2O3
It is the material of covalent bond type based on silicon nitride, thus during hot pressed sintering, causes Sialon ceramics to be difficult to Fine and close.After inserting sintering aid in the feed, during hot pressed sintering, part sintering aid is changed by solid phase For liquid phase, thus improved the compactness of the Sialon ceramics target obtained by liquid-phase sintering.
In the present embodiment, the preferred Y of described sintering aid2O3.Described Y2O3After liquid phase, other are former with part Material reaction, and make Y2O3It is liquid phase or molten condition with other raw materials of part, fine and close with acceleration of sintering.
Described conductive agent can improve the electric conductivity of the Sialon ceramics target of acquisition.Described conductive agent is chosen as Metallic compound, is chosen as metal nitride, further such as TiN and TaN.In sintering process, lead Electricity agent can be connected with each other with raw material components such as aluminium nitride, silicon nitride by " metal-N " key, becomes pottery Stable phase in target.
In the present embodiment, described conductive agent is TiN.
In the present embodiment, in described material powder, silicon nitride, aluminium oxide, aluminium nitride, sintering aid and The weight content of conductive agent is: 45~60wt%, 2~10wt%, 2~5wt%, 5~10wt%, 30~45wt%. Concrete ratio makees concrete configuration according to the performance of the Sialon ceramics being actually needed acquisition.
In the present embodiment, in described material powder, the grain diameter of each component is chosen as 2~3 μm.
With continued reference to shown in Fig. 1, perform step S2, by material powder mix homogeneously.
In the present embodiment, the hybrid technique used is chosen as ball-milling technology.
Wherein Fig. 2 illustrates ball-milling technology, specifically includes: described material powder 10 is placed in ball grinder 20 In, after described ball grinder 20 inserts disperse medium (not shown) and ball-milling medium 30, ball Mill 16~24h, makes each component mix homogeneously in described material powder 10.
Described ball-milling medium 30 particle diameter is far longer than each material powder particle diameter, in mechanical milling process, rocks described Ball grinder 20 so that ball-milling medium 30 fully stirs in described material powder 10, so that raw material Each component mix homogeneously in powder.Described ball-milling medium 30 is chosen as aluminium oxide and zirconium oxide.
In the present embodiment, described ball-milling medium 30 is zirconium oxide.
Described disperse medium is chosen as alcohols, arene etc. and has less capillary material, described Alcohols includes that ethanol, glycerol etc., described arene material include benzene, toluene etc..In mechanical milling process, Described disperse medium can effectively reduce each intergranular adhesiveness in material powder, thus effectively dispersion is each The little granule of raw material so that in material powder, the mixing of each component is more uniformly distributed.
In the present embodiment, described disperse medium is dehydrated alcohol, glycerol or both mixture.
After each for described material powder component being sufficiently mixed, it is dried process, is used for removing described ball The disperse medium added in described material powder 10 in grinding process, thus obtain the material powder being dried.
The temperature that described dry treatment process is used is less than the boiling point of disperse medium, in dried process In make disperse medium slowly volatilize, it is to avoid based on disperse medium boiling and cause raw material mixing uneven, from And equipment causes damage, and cause Sialon ceramics target processing technology more loaded down with trivial details.
In the present embodiment, use dehydrated alcohol, glycerol or both mixture as disperse medium, institute The temperature stating dry treatment process employing is 70~80 DEG C.
With continued reference to shown in Fig. 1, after dried obtains the material powder being dried, perform step S3, Carry out hot pressed sintering process, form Sialon ceramics target.
The concrete process using hot pressed sintering to process technique formation Sialon ceramics target is with reference to Fig. 3 and Fig. 4.
As it is shown on figure 3, after dried material powder 10 is loaded graphite jig 40, by described graphite Mould 40 is placed in vacuum sintering funace 50, carries out hot pressed sintering process.Wherein, described graphite mo(u)ld Has 40 structures configuration settings according to Sialon ceramics target to be formed.
As shown in Figure 4, after hot pressed sintering processes, prepare Sialon ceramics target 11.
Specifically, described hot pressed sintering process technique includes:
The early stage temperature rise period: initiateed intensification by room temperature, regulate the heating of described vacuum sintering funace 50 Speed is 5~10 DEG C/min, until the temperature of described vacuum sintering funace 50 up to 1200 DEG C.This stage In, material powder form do not have the biggest change, can make former with the rate of heat addition of 5~10 DEG C/min Material powder each component thermally equivalent, stable intensification;
Afterwards, enter the temperature rise period in mid-term, regulate the rate of heat addition of described vacuum sintering funace 50 1.5~3 DEG C/min, it is chosen as 2 DEG C/about min.Relative to the described early stage temperature rise period, in this stage, Slow down the heating rate of vacuum sintering funace, until 1300~1400 DEG C.Gradually heat up after 1200 DEG C During, Si3N4Starting phase transformation occur, during this, the speed of heating of 1.5~3 DEG C/min can make part α-Si3N4Fully it is transformed into β-Si3N4, other components and α-Si3N4With β-Si3N4α is included in conjunction with formation The Sialon ceramics target of-sialon and β-sialon, and the most also can be effectively improved TiN and The bond strength of other components, to improve the performance of Sialon ceramics target.
In temperature rise period in mid-term, concrete intensification terminal and heating rate can according in material powder, Depending on the content of each component.
Finally, the temperature rise period in later stage is entered.Specifically, Si after 1300~1400 DEG C3N4Complete phase transformation Convert, in risen to the later stage temperature-rise period of 1400~1700 DEG C by 1300~1400 DEG C, the speed that heats up can be accelerated Rate, is heated to heat preservation sintering temperature 1450~1700 DEG C with the hot speed of 4~6 DEG C/min so that each group of raw material Divide fully heating.
And gradually risen by room temperature to heat preservation sintering temperature course, the most progressively strengthen hot pressed sintering Pressure in stove 50, until the pressure in described hot-pressed sintering furnace 50 is to presetting pressure.
In the present embodiment, described default pressure more than 20MPa just can, be chosen as 20~30MPa further, Described compression rate is controllable to 0.3~0.5MPa/min, at continuous pressure dwell, can effectively remove raw material The gas produced in middle temperature-rise period, the most progressively pressurization realizes raw material compacting, thus is effectively improved final The compactness of the Sialon ceramics target formed.
When the temperature in described vacuum sintering funace 50 up to 1450~1700 DEG C, pressure reaches to preset pressure Qiang Hou, heat-insulation pressure keeping heating 4~7h, thus form Sialon ceramics target.
During hot pressed sintering, after yittrium oxide forms liquid phase or molten state with other raw material components of part, Silicon nitride reacts with aluminium oxide and aluminium nitride, and the Si-N in silicon nitride is replaced by Al-O, and Si-N is by Al-N Replace, and later replaces uneven ruthenium ion of the electricity price caused and compensates, thus form Sialon ceramics. Titanium nitride is then evenly distributed in Sialon ceramics, can be effectively improved leading of prepared Sialon ceramics target Electrically and heat conductivity.
Under the conditions of more than 1700 DEG C, silicon nitride decomposes can become the form such as silicon oxide and nitrogen, no Reduced by only other component reaction in silicon nitride and material powder and form the probability of Sialon ceramics, and nitrogen Appearance can reduce the consistency of grand ceramic target.In the present embodiment, under the conditions of 1450~1700 DEG C, join Close and be processed operation under the pressure more than 20MPa, while guaranteeing to obtain Sialon ceramics target, have Effect inhibits silicon nitride to decompose, thus improves the quality of the Sialon ceramics target of acquisition.
By the above-mentioned step progressively heating up, boosting, in the present embodiment, only need to be 1450~1700 DEG C of conditions Under, more than heat-insulation pressure keeping heating 4~7h under conditions of 20MPa, just can obtain consistency and be up to 99%(survey Method for testing: GB3850-83 ≈ ISO3369-1975, dense sintering metal material is surveyed with hard alloy density Determine method) high-compactness Sialon ceramics target, it complies fully with magnetron sputtering requirement.Compared to existing Some temperature reach more than 1900 DEG C, and pressure reaches the hot pressed sintering of 50~60MPa and makes Sialon ceramics target The technique of material, the present embodiment greatly reduces the cost of manufacture of Sialon ceramics target, and for equipment Requirement.
In the present embodiment, in described hot pressed sintering processing procedure, also can be to described vacuum heating-press sintering It is passed through protective atmosphere, to strengthen the stability of hot pressed sintering processing procedure in stove 50.
Described protective atmosphere is chosen as nitrogen, argon, helium etc..
In the present embodiment, described protective gas is preferably nitrogen.Hot conditions during hot pressed sintering Under, silicon nitride there will be decomposition reaction and generates the component such as nitrogen and silicon oxide.Burning to described vacuum hotpressing After being passed through nitrogen in freezing of a furnace 50, can by strengthen nitrogen content promote silicon nitride resolve into generation nitrogen and The molecular balance of silicon oxide is carried out to reverse direction, and suppression silicon nitride resolves into the reaction of nitrogen and silicon oxide. Thus reduce the gas flow in reaction system, it is to avoid there are the defects such as pin hole in the Sialon ceramics target of formation, Thus improve the consistency of the Sialon ceramics target of formation.
It should be noted that in other embodiments, more described graphite jig 40 is placed in vacuum hotpressing burning Before freezing of a furnace 50 carries out hot pressed sintering, can first the material powder 10 in described graphite jig 40 be carried out Cold pressing treatment in advance, improves the compactness between material powder 10 in advance.
The Sialon ceramics target 11 that the manufacture method of the Sialon ceramics target provided by the present embodiment is prepared, Its consistency is up to 99%(method of testing: GB3850-83 ≈ ISO3369-1975, dense sintering metal Material and hard alloy density measurement method), and there is good conduction, heat conductivility.Thus at filament In cutting technique, the spark strengthening the constantly pulse feature of generation between Sialon ceramics target 11 and wire electrode is put Electrical effect, to accelerate the ablation of Sialon ceramics target 11 and the contact site of wire electrode, thus improves cutting The smoothness of Sialon ceramics target 11, is effectively improved the cutting performance of Sialon ceramics target 11, Jin Erti The machining accuracy of high Sialon ceramics target 11.
Although present disclosure is as above, but the present invention is not limited to this.Any those skilled in the art, Without departing from the spirit and scope of the present invention, all can make various changes or modifications, therefore the guarantor of the present invention The scope of protecting should be as the criterion with claim limited range.

Claims (11)

1. the manufacture method of a Sialon ceramics target, it is characterised in that including:
The material powder including silicon nitride, aluminium oxide, aluminium nitride, sintering aid and conductive agent is provided;Institute Stating conductive agent is titanium nitride or tantalum nitride;Described silicon nitride, aluminium oxide, aluminium nitride, sintering aid and lead The weight content of electricity agent is: 45~60wt%, 2~10wt%, 2~5wt%, 5~10wt%, 30~45wt%;
After described material powder mix homogeneously, carry out hot pressed sintering process, form Sialon ceramics target.
The manufacture method of Sialon ceramics target the most according to claim 1, it is characterised in that described hot pressing Sintering processes technique includes:
It is heated to 1200 DEG C with the speed of 5~10 DEG C/min;
Afterwards, it is heated to 1300~1400 DEG C with the speed of 1.5~3 DEG C/min;
Afterwards, it is heated to 1450~1700 DEG C with the speed of 4~6 DEG C/min;
With 0.3~0.5MPa/min speed persistent pressure, to presetting pressure, described default pressure is more than 20MPa;
And be 1450~1700 DEG C in temperature, preset heat-insulation pressure keeping heating 4~7h under pressure conditions.
The manufacture method of Sialon ceramics target the most according to claim 2, it is characterised in that described default Pressure is more than 20MPa and less than or equal to 30MPa.
The manufacture method of Sialon ceramics target the most according to claim 1, it is characterised in that described hot pressing Sintering processes is carried out under protective atmosphere.
5. the manufacture method of the Sialon ceramics target stated according to claim 4, it is characterised in that described protection gas Atmosphere includes Ar, He or N2Atmosphere.
The manufacture method of Sialon ceramics target the most according to claim 1, it is characterised in that by raw material powder The method of end mix homogeneously is ball-milling technology.
The manufacture method of Sialon ceramics target the most according to claim 6, it is characterised in that described ball milling Technique includes:
Described material powder is placed in ball grinder, after inserting disperse medium, ball milling 16~24h.
The manufacture method of Sialon ceramics target the most according to claim 7, it is characterised in that described ball milling Technique includes: using zirconium oxide or aluminium oxide as ball-milling medium.
The manufacture method of Sialon ceramics target the most according to claim 7, it is characterised in that described dispersion Medium is dehydrated alcohol and/or glycerol.
The manufacture method of Sialon ceramics target the most according to claim 9, it is characterised in that also include: After described ball-milling technology, described material powder is dried process.
The manufacture method of 11. Sialon ceramics targets according to claim 10, it is characterised in that described dry The temperature processed is less than the boiling point of disperse medium.
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Application publication date: 20150318

Assignee: NINGBO JIANGFENG ELECTRONIC MATERIAL CO., LTD.

Assignor: Ningbo Jiangfeng Powder Metallurgy Co., Ltd

Contract record no.: X2019330000048

Denomination of invention: Sialon ceramic target material production method

Granted publication date: 20161228

License type: Exclusive License

Record date: 20191203

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Address after: 315400 no.198 Anshan Road, Yuyao City, Ningbo City, Zhejiang Province

Patentee after: Ningbo Jiangfeng hot isostatic pressing technology Co.,Ltd.

Address before: 315400 no.198 Anshan Road, Yuyao City, Ningbo City, Zhejiang Province

Patentee before: Ningbo Jiangfeng Powder Metallurgy Co.,Ltd.

CP01 Change in the name or title of a patent holder