阅读说明：本技术 氮化铝掺氮化钪靶材的生产工艺 (Production process of aluminum nitride scandium-doped nitride target material ) 是由 吴文斌 舒小敏 于 2019-10-13 设计创作，主要内容包括：本发明公开了一种氮化铝掺氮化钪靶材的生产工艺,将高纯钪金属和铝金属粉末冷压成疏松块状,分别装入坩埚,移入真空加热炉,抽真空,通入氮气,采用程度升温气固合成法分别合成ScN、AlN,破碎、球磨成-100目粉末。ScN、AlN粉末检验合格后,按规定比例混合,以此为原料进行热压烧结,制得氮化铝掺氮化钪靶坯。对靶坯进行机械加工得到靶材。本发明采用程序升温气固合成技术分别合成氮化铝、氮化钪,制成粉末,然后通过真空热压烧结成型技术,制备规定比例的氮化铝掺氮化钪靶材,制备出的氮化铝掺氮化钪靶材是SAW厂家制备Sc掺杂氮化铝功能薄膜的前端产品,质量好、性能优异。(The invention discloses a production process of an aluminum nitride scandium-doped target material, which comprises the steps of cold-pressing high-purity scandium metal and aluminum metal powder into loose blocks, respectively filling the loose blocks into crucibles, respectively moving the crucibles into a vacuum heating furnace, vacuumizing, introducing nitrogen, respectively synthesizing ScN and AlN by adopting a temperature-rising gas-solid synthesis method, crushing and ball-milling into powder of-100 meshes. And after the ScN powder and the AlN powder are qualified, mixing the ScN powder and the AlN powder according to a specified proportion, and performing hot-pressing sintering on the mixture serving as a raw material to prepare the aluminum nitride scandium nitride target blank. And machining the target blank to obtain the target material. The method adopts a temperature programmed gas-solid synthesis technology to respectively synthesize aluminum nitride and scandium nitride to prepare powder, and then adopts a vacuum hot-pressing sintering molding technology to prepare the aluminum nitride scandium nitride target material with specified proportion, and the prepared aluminum nitride scandium nitride target material is a front-end product of a Sc doped aluminum nitride functional film prepared by an SAW manufacturer, and has good quality and excellent performance.)

1. A production process of an aluminum nitride scandium-doped target material is characterized by comprising the following steps:

the temperature programmed gas-solid synthesis technology respectively synthesizes aluminum nitride and scandium nitride,

i, AlN synthesis, namely, cold-pressing aluminum powder with the purity of more than 99.99 percent into loose blocks, filling the loose blocks into a crucible, moving the crucible into a vacuum heating furnace, vacuumizing to 1 ~ 5Pa, introducing nitrogen to 100 ~ 200kPa, heating to 500 ~ 600⁰C, preserving the temperature for 0.5h, and removing oxides on the surface of the aluminum powder;

heating is continued to 800 ~ 850⁰C, preserving heat for 1 ~ 2h to ensure that the aluminum powder and the nitrogen fully react, cooling to room temperature along with the furnace, taking out the synthesized product, crushing, ball-milling, repeating the process at 1100 ~ 1200⁰C, nitriding for 0.5h for the second time, cooling along with the furnace, and performing XRD test, wherein no impurity phase except the AlN phase is qualified;

crushing and ball-milling the qualified product to-300 meshes of AlN powder for later use;

II, synthesizing ScN, namely cold-pressing scandium powder with the purity of more than 99.99 percent into loose blocks, filling the loose blocks into a crucible, moving the crucible into a vacuum heating furnace, vacuumizing to 1 ~ 5Pa, introducing nitrogen to 100 ~ 200kPa, and heating to 800 ~ 900⁰C, preserving heat for 1 ~ 2h to ensure that scandium powder and nitrogen fully react, cooling to room temperature along with the furnace, taking out a synthetic product, crushing, ball-milling, cooling along with the furnace, and performing XRD test, wherein no impurity phase except the ScN phase is qualified;

if non-nitrided scandium metal exists, secondary nitridation is needed;

crushing and ball-milling the qualified product to-300-mesh ScN powder for later use;

(2) hot pressing, sintering and forming, namely filling the prepared powder into a die according to the calculated dosage of theoretical proportion, transferring into a vacuum hot pressing furnace, and sintering and forming at the sintering temperature of 1500 ~ 1600⁰C, applying pressure of 12 ~ 25MPa, and sintering for 30 ~ 80min to obtain a blank of the aluminum nitride scandium-doped target material;

(3) and testing the structure, the components and the like of the prepared target, forming a film by magnetron sputtering, and obtaining the quality information of the target through film performance testing.

2. The production process of the aluminum nitride scandium-doped target material according to claim 1, characterized by further comprising the following steps: carrying out heat treatment on the aluminum nitride scandium nitride blank formed by hot-pressing sintering at the heat treatment temperature of 0.4Tm, and then carrying out mechanical processing procedures such as water cutting, cylindrical grinding, plane grinding, machine tool processing, polishing and the like to prepare a marketable target material;

the indexes are as follows:

1) and a relative density of 99% or more;

2) the purity is more than 99.99 percent, and the sum of the contents of main impurities is less than 100 mu g/g;

3) the grain size is less than or equal to 50 mu m.

Technical Field

The invention relates to the technical field of production of aluminum nitride scandium nitride targets, and relates to a production technology of an aluminum nitride scandium nitride target.

Background

The piezoelectric thin film material is a key material for preparing a thin film Surface Acoustic Wave (SAW) device, and the performance of the piezoelectric thin film material determines the performance of the SAW device. The aluminum nitride is a good piezoelectric film material, has the advantages of high acoustic wave speed, high thermal conductivity, low dielectric loss, excellent temperature stability, compatibility with a CMOS (complementary metal oxide semiconductor) process and the like, and is an ideal material for preparing high-frequency, high-power and high-integration SAW devices. The ScN is doped into the AlN (which is different from Sc doped AlN), so that the lower piezoelectric coefficient and electromechanical coupling coefficient of the AlN can be effectively improved, and the performance of the AlN as a piezoelectric thin film material is improved, thereby preparing the SAW device with more excellent performance. At present, the Sc doped AlN thin film is prepared at home and abroad mostly in a reactive sputtering mode, an aluminum scandium metal target material is put into reactive sputtering equipment, and argon and nitrogen are introduced after vacuum pumping, wherein the argon is a working gas, and the nitrogen is a reaction gas. Under the action of electromagnetism, ionized argon positive ions bombard the surface of an aluminum-scandium metal target along a direction with a certain included angle, aluminum-scandium metal components escape from the surface of the target, fly out along the symmetrical direction of the bombardment direction and fly to the surface of a base material, and the aluminum-scandium metal reacts with nitrogen in the sputtering process to generate AlN and ScN which are deposited on the surface of the base material and crystallized to form a layer of functional film. The method for preparing the film in the reactive sputtering mode has the advantages that both sputtering coating and chemical combination reaction are considered, the two aims are achieved, the preparation conditions are difficult to control, such as the difference of the reaction conditions of aluminum, scandium and nitrogen, the difference of the reaction conditions and the sputtering conditions, the problem of nitrogen guest series working gas and the like, and the difference, the problem and the derived deep-level problem are comprehensively considered. Although a comprehensive optimal set of operating parameters can be obtained through research, the reaction and sputtering must be compatible, and certain disadvantages which are difficult to overcome are inevitable. For example, the target material poisoning phenomenon in the preparation process, incomplete nitridation metal impurities or low-valence nitrides may exist in the film, the film may have a partially amorphous state, the morphology of the film may be unsatisfactory, and the like, thereby causing many disadvantages such as increased cost, reduced production efficiency, and poor film performance.

Disclosure of Invention

In order to overcome the defects of the prior art, the invention provides a production process of an aluminum nitride scandium-doped target material. Aluminum nitride and scandium nitride are respectively synthesized by adopting a temperature programmed gas-solid synthesis technology to prepare powder, and then the aluminum nitride scandium nitride target material with specified proportion is prepared by adopting a vacuum hot-pressing sintering molding technology.

The invention relates to a production process of a zinc telluride doped cuprous telluride target material, which comprises the following steps:

(1) respectively synthesizing aluminium nitride and scandium nitride by programmed heating gas-solid synthesis technology

I, AlN synthesis, namely, cold-pressing aluminum powder with the purity of more than 99.99 percent into loose blocks, filling the loose blocks into a crucible, moving the crucible into a vacuum heating furnace, vacuumizing to 1 ~ 5Pa, introducing nitrogen to 100 ~ 200kPa, heating to 500 ~ 600⁰C, preserving the heat for 0.5h, removing the oxide on the surface of the aluminum powder, and continuing heating to 800 ~ 850⁰C, preserving heat for 1 ~ 2h to ensure that the aluminum powder and the nitrogen fully react, cooling to room temperature along with the furnace, taking out the synthesized product, crushing, ball-milling, repeating the process at 1100 ~ 1200⁰C is nitrided for 0.5h for the second time, cooled along with the furnace, and subjected to XRD test, and the product is qualified without impurity phases except AlN phases. And crushing and ball-milling the qualified product to-300-mesh AlN powder for later use.

II, synthesizing ScN, namely cold-pressing scandium powder with the purity of more than 99.99 percent into loose blocks, filling the loose blocks into a crucible, moving the crucible into a vacuum heating furnace, vacuumizing to 1 ~ 5Pa, introducing nitrogen to 100 ~ 200kPa, and heating to 800 ~ 900⁰And C, preserving heat for 1 ~ 2h to ensure that scandium powder and nitrogen fully react, cooling to room temperature along with the furnace, taking out a synthesized product, crushing, ball-milling, cooling along with the furnace, performing XRD test, judging that no impurity phase except the ScN phase is qualified, performing secondary nitridation if non-nitrided scandium metal exists, crushing the qualified product, and ball-milling to-300-mesh ScN powder for later use.

(2) Hot pressed sintering forming

The prepared powder is loaded into a die according to the calculated dosage in advance according to the theoretical proportion, and is moved into a vacuum hot pressing furnace for sintering and forming, wherein the sintering temperature is 1500 ~ 1600⁰And C, applying pressure of 12 ~ 25MPa, and sintering for 30 ~ 80min to obtain the aluminum nitride scandium nitride target blank.

(3) And testing the structure, the components and the like of the prepared target, forming a film by magnetron sputtering, and obtaining the quality information of the target through film performance testing.

Further, the method also comprises the following steps: the aluminum nitride scandium nitride blank formed by hot-pressing sintering is subjected to heat treatment at the temperature of 0.4Tm, and then is subjected to mechanical processing procedures such as water cutting, cylindrical grinding, plane grinding, machine tool processing, polishing and the like to prepare the marketable target material. The size can be according to the requirement of the client. The indexes are as follows:

1) and a relative density of 99% or more;

2) the purity is more than 99.99 percent, and the sum of the contents of main impurities is less than 100 mu g/g;

3) the grain size is less than or equal to 50 mu m.

The invention adopts a temperature programmed gas-solid synthesis technology to respectively synthesize aluminum nitride and scandium nitride to prepare powder, then prepares an aluminum nitride scandium-doped target material with specified proportion by a vacuum hot-pressing sintering molding technology, the prepared aluminum nitride scandium-doped target material is a front-end product of a Sc-doped aluminum nitride functional film prepared by an SAW manufacturer, and provides the aluminum nitride scandium-doped target material product for the SAW manufacturer, the SAW manufacturer can use the aluminum nitride scandium-doped target material to carry out magnetron sputtering coating, and the problem of reaction of aluminum scandium and nitrogen is not required to be considered while coating, thus the method for preparing the film has the advantages of easily controllable and stable preparation conditions, simple mechanism in the preparation process, uniform and compact components, good quality and excellent performance of the prepared film.

Detailed Description