CN102337506B - Manufacturing method of silver alloy sputtering target - Google Patents

Abstract

The invention relates to a manufacturing method of a silver alloy sputtering target, which comprises the steps of: strictly controlling a material distribution proportion and a feeding sequence, and strictly controlling the smelting temperature and the smelting duration of the alloy components in the smelting and refining processes to obtain an alloy target material capable of replacing a silver target material in the prior art and capable of overcoming the technical defects of the silver target material, namely, the obtained alloy sputtering target is entitled with excellent performance by distributing different smelting temperatures and smelting durations on alloys with different components.

Description

A kind of method of manufacture of silver alloy sputtering target

Technical field

The invention relates to a kind of method of manufacture of silver alloy sputtering target.

Background technology

The film that the fine silver sputtering target forms, owing to have high-reflectivity and low-resistance characteristic, so be applicable to the reflectance coating of optical record medium, the electrode reflectance coating of reflection LCD etc.

But on the one hand it is with high costs for the fine silver sputtering target; The film of fine silver sputtering target formation is being exposed under the airborne situation for a long time or is being exposed under the hot and humid situation on the other hand; The surface oxidation easily of film; Produce phenomenons such as silver-colored crystal grain-growth or silver atoms cohesion in addition, can produce the deterioration of electroconductibility and the decline of reflectivity thus, or make the problems such as cementability deterioration with substrate.Thereby, examination recently on one side carried out much about keep the original high reflectivity of fine silver, by the improvement of interpolation alloying element raising its erosion resistance.And; When carrying out such film improvement; Also study forming the employed target of silver alloy film; For example, open in the 2001-192752 communique the spy and to disclose a kind of following sputtering target as one of electronic component-use metallic substance, it is staple with Ag; And contain the Pd of 0.1～3wt% in order to improve weathering resistance, further in order to suppress owing to the increase of adding the caused resistivity of Pd contains a plurality of elements 0.1～3wt% scope, that from the crowd who is made up of Al, Au, Pt, Cu, Ta, Cr, Ti, Ni, Co, Si etc., select.

Summary of the invention

The present invention makes in view of the above problems, and its purpose is to provide to be beneficial to by sputtering method and forms the method for manufacture that thickness and one-tenth are grouped into uniform silver alloys target.

The method of manufacture of the application's silver alloy sputtering target comprises the steps:

Step 1, batching: according to furnace capacity, go out the input weight of each alloy constituent element according to the alloying constituent percentage calculation, each constituent element calculates according to mass percent; Zr is that 0.3-2.5%, Re are that 0.02-1%, Ag are 0.05-0.5%, and surplus is Al;

Step 2, feed intake: feeding sequence Al, AlZr alloy, AlAg alloy, AlRe alloy;

Step 3, melting: smelting temperature is Al 680-710 ℃, 700-740 ℃ of AlZr alloy, 740 ℃ of AlAg alloys; 700-730 ℃ of AlRe alloy, wherein smelting time is: Al 10-60 minute, AlZr alloy 10-15 minute; AlAg alloy 15-20 minute, AlRe alloy 5-10 minute;

Step 4, refining: refining agent is sent into furnace bottom through pure carbon tube by argon gas, fully stir, degasification is skimmed, and leaves standstill 10 minutes;

Step 5, casting: make cylinder iron or the cast steel metal die extrusion molding of casting;

Step 6, thermal treatment: 300-420 ℃ homogenizing annealing 2 hours.

Used refining agent is this area commercially available refining agent commonly used, such as SODIUMNITRATE or Sesquichloratum.

The inventor is through a large amount of secular experiments; Discovery is according to above-mentioned proportion scale and feeding sequence; And in melting and refining process the alloy target material that smelting temperature and smelting time obtained of strict each alloy constituent element of control; Silver-colored target of the prior art can be replaced fully, and the existing technological deficiency of silver-colored target can be overcome.That is, cooperate different smelting temperature and smelting time, make the alloy sputtering target of acquisition have excellent performance through alloy to different components.

The contriver has carried out spectral detection to the sputtering target that is made by aforesaid method, uses instrument to be ICP-OES.

The pre-treatment analytical procedure:

One, sample preparation: the pollution-free part of extraction sample is pulverized or is stirred, and the sample sack of packing into is with to be analyzed.

Two, clear up sample

Usually take by weighing 0.1 to 0.2 gram sample and clear up, the method for degestion appearance has three kinds usually.

(1) sour degestion mainly to the pure metal sample, requires sample to be dissolved in the acid solution fully.

(2) dry ashing method mainly to nonmetal flammable sample, with the high-temperature sample ashing, adds acid dissolving with retort furnace again, and tested element can both be dissolved in the acid, requires the metal ingredient loss that can not in high temperature, distil.

(3) Microwave Digestion, this method will use microwave dissolver.This method is practiced thrift reagent, and it is best to clear up effect, but speed is slower, and in addition, speed is separated sample can not use this method, to avoid explosion accident.

Three, cleared up after the sample, filtered and the constant volume sample.

The step of using ICP-OES that sample is analyzed is following: sets up testing method, sets up typical curve testing standard sample with standardized solution typical curve is tested, and specimen, the arrangement result provides report.

Reflection: opticinstrument

Use instrument: microphotometer, test procedure: sample preparation, after the sample polishing, should be placed in the moisture eliminator 10h or spend in the baking oven of 40 degree and place 4 hours 30, can be used for test.The oil immersion drop is placed on the microscope carrier flattening on the sample polished surface on the slide glass and with sample, and whether modulated Cheng Ke reins in illumination to the inspection microscope lamp.Calibrating instrument is chosen the reference material of two reflectivity and sample and is demarcated, and shows that the difference of reading and standard value can not can be measured sample greater than 2%.Working sample.The establishment report.

The analysis of grain-size: use instrument to be metallographic polisher lapper, metaloscope.Step: sample preparation, process the square of 20mm*20mm*20mm through cutting sample usually.Sample is ground, should use the water law sandpaper during grinding, and thin by being milled to, and note the smooth of abrasive surface.Sample is polished.Prepare suitable etching reagent, sample is corroded, etching time should be suitable, obviously is as the criterion with crystal grain in microscope.In metaloscope, observe, be adjusted to rational magnification, take pictures at the most clear position of crystal grain according to grain size.In (5), under the identical multiple scale is taken pictures (being used to contrast grain-size).Make the metallurgical analysis report with crystalline phase figure and scale map.

Sputtering target by the application's preparation can be used to prepare CD reflection layer, the plated film functional film layer that substitutes silver.With the prior art correlation data:

Embodiment

Below further describe the present invention through embodiment, but the present invention is not limited only to following embodiment.

Embodiment 1

The method of manufacture of silver alloy sputtering target comprises the steps:

Step 1, batching: according to furnace capacity, go out the input weight of each alloy constituent element according to the alloying constituent percentage calculation, each constituent element calculates according to mass percent; Zr is 0.3%, Re is 0.02%, Ag is 0.05%, and surplus is Al;

Step 2, feed intake: feeding sequence Al, AlZr alloy, AlAg alloy, AlRe alloy;

Step 3, melting: smelting temperature is 680 ℃ of Al, 700 ℃ of AlZr alloys, and 740 ℃ of AlAg alloys, 700 ℃ of AlRe alloys, wherein smelting time is: Al 10 minutes, AlZr alloy 10 minutes, AlAg alloy 15 minutes, AlRe alloy 5 minutes;

Step 4, refining: refining agent is sent into furnace bottom through pure carbon tube by argon gas, fully stir, degasification is skimmed, and leaves standstill 10 minutes;

Step 5, casting: make cylinder iron or the cast steel metal die extrusion molding of casting;

Step 6, thermal treatment: 300 ℃ of homogenizing annealings 2 hours.

Embodiment 2

The method of manufacture of silver alloy sputtering target comprises the steps:

Step 1, batching: according to furnace capacity, go out the input weight of each alloy constituent element according to the alloying constituent percentage calculation, each constituent element calculates according to mass percent; Zr is 2.5%, Re is 1%, Ag is 0.5%, and surplus is Al;

Step 2, feed intake: feeding sequence Al, AlZr alloy, AlAg alloy, AlRe alloy;

Step 3, melting: smelting temperature is Al710 ℃, 740 ℃ of AlZr alloys, and 740 ℃ of AlAg alloys, 730 ℃ of AlRe alloys, wherein smelting time is: Al 60 minutes, AlZr alloy 15 minutes, AlAg alloy 20 minutes, AlRe alloy 10 minutes;

Step 4, refining: refining agent is sent into furnace bottom through pure carbon tube by argon gas, fully stir, degasification is skimmed, and leaves standstill 10 minutes;

Step 5, casting: make cylinder iron or the cast steel metal die extrusion molding of casting;

Step 6, thermal treatment: 420 ℃ of homogenizing annealings 2 hours.

Embodiment 3

The method of manufacture of silver alloy sputtering target comprises the steps:

Step 1, batching: according to furnace capacity, go out the input weight of each alloy constituent element according to the alloying constituent percentage calculation, each constituent element calculates according to mass percent; Zr is 2.0%, Re is 0.06%, Ag is 0.10%, and surplus is Al;

Step 2, feed intake: feeding sequence Al, AlZr alloy, AlAg alloy, AlRe alloy;

Step 3, melting: smelting temperature is 690 ℃ of Al, 720 ℃ of AlZr alloys, and 740 ℃ of AlAg alloys, 720 ℃ of AlRe alloys, wherein smelting time is: Al 30 minutes, ALZr alloy 15 minutes, AlAg alloy 15 minutes, AlRe alloy 8 minutes;

Step 4, refining: refining agent is sent into furnace bottom through pure carbon tube by argon gas, fully stir, degasification is skimmed, and leaves standstill 10 minutes;

Step 5, casting: make cylinder iron or the cast steel metal die extrusion molding of casting;

Step 6, thermal treatment: 380 ℃ of homogenizing annealings 2 hours.

Claims (1)

1. the method for manufacture of a silver alloy sputtering target is characterized in that:

Step 1, batching: according to furnace capacity, go out the input weight of each alloy constituent element according to the alloying constituent percentage calculation, each constituent element calculates according to mass percent; Zr is that 0.3-2.5%, Re are that 0.02-1%, Ag are 0.05-0.5%, and surplus is Al;

Step 2, feed intake: feeding sequence Al, AlZr alloy, AlAg alloy, AlRe alloy;

Step 3, melting: smelting temperature is respectively Al 680-710 ℃, 700-740 ℃ of AlZr alloy, 740 ℃ of AlAg alloys; 700-730 ℃ of AlRe alloy, wherein smelting time is: Al 10-60 minute, AlZr alloy 10-15 minute; AlAg alloy 15-20 minute, AlRe alloy 5-10 minute;

Step 4, refining: refining agent is sent into furnace bottom through pure carbon tube by argon gas, fully stir, degasification is skimmed, and leaves standstill 10 minutes;

Step 5, casting: make cylinder iron or the cast steel metal die extrusion molding of casting;

Step 6, thermal treatment: 300-420 ℃ homogenizing annealing 2 hours.