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Preparing method of high-densification ultra-fine grain large-size molybdenum target

An ultra-fine-grained, large-size technology, applied in metal material coating process, vacuum evaporation plating, coating, etc., can solve the problems of insufficient density, particle splashing, coarse grains of molybdenum billet metal, etc., to improve the thin film performance, increased sputtering speed, and improved quality

Active Publication Date: 2019-05-21
安泰天龙钨钼科技有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there are many methods for preparing molybdenum targets for sputtering coatings, such as sintering, electron beam smelting, hot isostatic pressing, etc., but each of the above methods has its own advantages and disadvantages, and none of them can well meet the needs of large-area coatings. Practical application needs
Among them, the cost of electron beam smelting is high, the operation is complicated, the smelted molybdenum billet metal grains are coarse, and subsequent processing is difficult, and it is difficult to ensure the fine and uniform grain structure required by the product target; the target produced by the sintering method has more hole defects , the density is insufficient, and the produced targets are prone to particle splashing and other problems during use; the hot isostatic pressing method cannot produce larger-sized targets, and according to relevant data, the length of the targets prepared by this method cannot exceed 2m
[0004] During the sputtering process, if the number of inclusions in the target is too large or the distribution is uneven, particles will often be formed on the wafer, resulting in uneven sputtering thickness or low sputtering efficiency, which seriously affects the film performance
In addition, the rate of thin film sputtering is related to the crystallization result and grain size of the molybdenum target. Molybdenum atoms are most likely to be preferentially sputtered along the direction of the hexagonal arrangement of atoms, and the sputtering rate of the fine-sized grain target is also relatively coarse. Grain target block, so increasing the sputtering rate of the molybdenum target and improving its quality can be achieved by changing the grain structure of the target, improving the purity of the target and refining the grain, but it has a preferred orientation for the preparation of the existing technology Molybdenum targets are very difficult, so the preparation of high-purity, fine-grained molybdenum targets has become an important research direction

Method used

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  • Preparing method of high-densification ultra-fine grain large-size molybdenum target
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  • Preparing method of high-densification ultra-fine grain large-size molybdenum target

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preparation example Construction

[0043] A method for preparing a high-density ultra-fine-grained large-size molybdenum target provided by the present invention comprises the following steps:

[0044] (1) cold isostatic pressing type

[0045] Select molybdenum powder, put the prepared molybdenum powder into the mold, and then put it into the cold isostatic pressing equipment for cold isostatic pressing, and obtain the cold isostatic pressing green body after pressure relief;

[0046] Preferably, the molybdenum content of the molybdenum powder is ≥99.95%, which meets the national standard GB / T3461-2006. The Fischer particle size is 3.0-3.8μm and the bulk density is 4.0-8.0g / cm 3 , and use a standard sieve to filter out the molybdenum powder with large particle size before using the molybdenum powder.

[0047] Preferably, the density of the cold isostatic pressed body after cold isostatic pressing is not lower than 40%.

[0048] (2) Sintering

[0049] The cold isostatic pressed green body is sintered by inducti...

Embodiment 1

[0072] The specifications of the finished molybdenum target prepared in the embodiment of the present invention are: length 3430 mm, width 400 mm, thickness 18 mm.

[0073] Such as figure 1 As shown, the preparation method of a high-density ultra-fine-grained large-size molybdenum target provided by the embodiment of the present invention includes the following steps:

[0074] (1) Molybdenum powder analysis and powder preparation

[0075] Use ICP atomic absorption spectrometer and carbon-oxygen analyzer to analyze the purity of molybdenum powder, requiring Mo content ≥ 99.5%, and controlling the content of impurity elements in the following range:

[0076] C<0.003; O<0.1; N<0.001; S<0.001; Fe<0.003; Sn<0.0005; Ni<0.003; Sb<0.01; Si<0.002; Cd<0.0005; Al<0.001; 0.002; Cu<0.001; W<0.02; Pb<0.0005; Bi<0.0005.

[0077] The particle size standard meets GB / T3461-2006 national standard, the Fischer particle size is 3.0-3.8μm, and the bulk density is 4.0-8.0g / cm 3 . Select molybde...

Embodiment 2

[0100] The specifications of the finished molybdenum target prepared in the embodiment of the present invention are: length 2300 mm, width 1800 mm, thickness 14 mm.

[0101] A method for preparing a high-density ultra-fine-grained large-size molybdenum target provided by an embodiment of the present invention includes the following steps:

[0102] (1) Molybdenum powder analysis and powder preparation

[0103] Use ICP atomic absorption spectrometer and carbon-oxygen analyzer to analyze the purity of molybdenum powder, requiring Mo content ≥ 99.5%, and controlling the content of impurity elements in the following range:

[0104] C<0.003; O<0.1; N<0.001; S<0.001; Fe<0.003; Sn<0.0005; Ni<0.003; Sb<0.01; Si<0.002; Cd<0.0005; Al<0.001; 0.002; Cu<0.001; W<0.02; Pb<0.0005; Bi<0.0005.

[0105] The particle size standard meets GB / T3461-2006 national standard, the Fischer particle size is 3.0-3.8μm, and the bulk density is 4.0-8.0g / cm 3 . Select molybdenum powder with a median value ...

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Abstract

The invention provides a preparing method of a high-densification ultra-fine grain large-size molybdenum target. According to the preparing method, through the processes of isostatic cool pressing profiling, sintering, hot isostatic pressing profiling, hot rolling, annealing and machining, the molybdenum target is prepared, the molybdenum target is subjected to hot isostatic pressing treatment, the molybdenum target blank is subjected to primary densification treatment, the blank is subjected to hot rolling treatment, the molybdenum target blank is subjected to secondary densification treatment, and finally, through procedures of annealing treatment, mechanical machining and the like at the temperature of 950 DEG C to 1100 DEG C and heat preservation for 60 to 90 min, the molybdenum targetwith the needed property is obtained. The preparing method can manufacture the molybdenum target with high purity (purity above 99.9%), full densification (density above 99.9%), and ultra-fine grains(grain size smaller than 20 micrometers), the sputtering technology with the higher and higher requirement can be met, the thin film sputtering speed is improved, the molybdenum metal sputtering thinfilm quality is improved, and the thin film property is improved.

Description

technical field [0001] The invention belongs to the technical field of sputtering target preparation, and in particular relates to a preparation method of a high-density ultra-fine grain large-size molybdenum target. Background technique [0002] In recent years, with the continuous development of technologies in the fields of solar cells, flat panel displays, and semiconductor integrated circuits, thin films deposited by sputtering have high density and good adhesion to substrate materials, so they have been widely used in these fields. Wide range of applications. Due to the low resistivity, strong thermal stability, good corrosion resistance and good environmental protection performance of molybdenum sputtered film, this film has broad market prospects in the fields of solar cells, flat panel displays, and semiconductor integrated circuits. [0003] At present, there are many methods for preparing molybdenum targets for sputtering coatings, such as sintering, electron bea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C14/34B22F5/00
Inventor 阚金锋钟铭杨义兵李旺李阳董建英王广达
Owner 安泰天龙钨钼科技有限公司
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